EP3094691A1 - Powder paint in particulate and hardened form having effect pigments and method for producing powder paint having effect pigments - Google Patents

Powder paint in particulate and hardened form having effect pigments and method for producing powder paint having effect pigments

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Publication number
EP3094691A1
EP3094691A1 EP15700490.4A EP15700490A EP3094691A1 EP 3094691 A1 EP3094691 A1 EP 3094691A1 EP 15700490 A EP15700490 A EP 15700490A EP 3094691 A1 EP3094691 A1 EP 3094691A1
Authority
EP
European Patent Office
Prior art keywords
effect pigments
powder coating
pigments
powder
effect
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
EP15700490.4A
Other languages
German (de)
French (fr)
Other versions
EP3094691B1 (en
Inventor
René MATTERN
Roman Büeler
Leo D'Anna
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
IGP Pulvertechnik AG
Original Assignee
IGP Pulvertechnik AG
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
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Application filed by IGP Pulvertechnik AG filed Critical IGP Pulvertechnik AG
Priority to PL15700490T priority Critical patent/PL3094691T3/en
Priority to EP15700490.4A priority patent/EP3094691B1/en
Publication of EP3094691A1 publication Critical patent/EP3094691A1/en
Application granted granted Critical
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Classifications

    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/32—Radiation-absorbing paints
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/0015—Pigments exhibiting interference colours, e.g. transparent platelets of appropriate thinness or flaky substrates, e.g. mica, bearing appropriate thin transparent coatings
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/62—Metallic pigments or fillers
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/62—Metallic pigments or fillers
    • C09C1/64—Aluminium
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/03—Powdery paints
    • C09D5/032—Powdery paints characterised by a special effect of the produced film, e.g. wrinkle, pearlescence, matt finish
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/29—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes for multicolour effects
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/80—Processes for incorporating ingredients
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D2401/00—Form of the coating product, e.g. solution, water dispersion, powders or the like
    • B05D2401/30—Form of the coating product, e.g. solution, water dispersion, powders or the like the coating being applied in other forms than involving eliminable solvent, diluent or dispersant
    • B05D2401/32—Form of the coating product, e.g. solution, water dispersion, powders or the like the coating being applied in other forms than involving eliminable solvent, diluent or dispersant applied as powders
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D5/00—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
    • B05D5/06—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures to obtain multicolour or other optical effects
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/51—Particles with a specific particle size distribution
    • C01P2004/52—Particles with a specific particle size distribution highly monodisperse size distribution
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00—Use of pretreated ingredients
    • C08K9/10—Encapsulated ingredients

Definitions

  • the present invention relates to a powder coating in partiku ⁇ L ⁇ rer and hardened form with effect pigments as well as methods for the preparation of powder paint with effect pigments.
  • effect pigments are used in powder coatings to achieve various optical effects.
  • Verschie ⁇ dene process for refining powder coatings with effect pigments and the corresponding provided with effect pigments powder coatings are known.
  • the simplest method is the so- ⁇ called "dry-blend" process, where an appropriate amount of Ef ⁇ Anlagenpigmenten is added to the final base powder coating and in a mixing process, a homogeneous distribution of the effect pigments is achieved in basic powder coating.
  • a disadvantage of this method is the lack of separation stability, which makes in particular ⁇ sondere in the processing of large quantities, for example in automated powder coating noticeable. Particularly in a large coated surface can result in a cloud-like appearance, caused by under ⁇ Kunststoffliches charging and deposition behavior between the powder particles and the dry admixed effect pigments, Other reasons include the different density between the powder coating particles and the effect pigments as well as the different particle size and particle shape.
  • This lack of separation stability makes the corresponding powder coatings only conditionally suitable for use in architecture example ⁇ example, for coating complex geometric, effective facade elements.
  • the powder coating obtained in this way is significantly more resistant to segregation compared to a powder coating obtained by the above-mentioned "dry-blend” process, but it is disadvantageous to carry out the complex and batch-only process and the difficult process control, thus making it possible to attach the effect pigments to the base powder incomplete.
  • a Se ⁇ are groomed between base powder and unattached effect means occurs during powder application, so that here too, albeit less pronounced than with Created in "dry-blend” process powder coating, a streaky or cloudy surface after Burning can result.
  • modified / stabilized effect ⁇ pigments on the market which are already surrounded by a bin ⁇ deffen GmbH.
  • these effect pigments alone are not yet film-forming.
  • Such modified avapig ⁇ elements must be added before the herstel ⁇ lung, the powder coating mixture according to manufacturer's instructions and as the usual chen powder coating ingredients are uniformly mixed and connected in an extruder by conventional extrusion.
  • demoei ⁇ lig of this process is in particular the fact that the effect pigments of extreme by the processing in the extruder
  • a powder coating is to be provided in particulate form, which is characterized in the application by a high segregation stability ⁇ net.
  • An inventive powder coating in particulate form with effect pigments is characterized in that the effect pigments are substantially wetted and coated with a film-forming coating matrix.
  • a powder coating is capable of film formation.
  • “wetted and coated essentially with the paint matrix” is understood to mean that the surface of the effect pigments is at least 50%, especially at least 75%, be ⁇ vorzugt at least 90% of paint occupied. Through this order ⁇ hüllung the effect pigments with the coating matrix can be ensured that the coated effect pigments in elektrostati ⁇ rule application have a similar charge and deposition behavior and so far very difficult can not segregate from the powder coating particles up.
  • the coating of the effect pigments with the lacquer matrix in the lacquer likewise ensures that a uniform effect can be achieved over the entire surface during subsequent application and subsequent stoving of the powder lacquer.
  • a paint matrix is understood to mean the mixed-together starting materials of the powder paint except the effect pigments.
  • the mixed-together starting materials of the powder coating form a thermosetting paint film after the baking process. Accordingly, a resist ⁇ matrix comprises all components which are necessary for the formation of a lacquer layer.
  • the paint matrix is therefore to be understood as identical to a paint.
  • At least 80%, especially at least 90%, preferably Wenig ⁇ least 95% of effect pigments can be Plated ⁇ gen with the paint matrix. This large amount of paint-coated effect pigments ensures easier handling of the Pulverla ⁇ ckes.
  • the determination of whether and what proportion of the effect pigments is coated with lacquer is carried out, for example, optically on a sample of the powder lacquer. It is important to ensure that the sample must be so large chosen so that a statistical statement is mög ⁇ Lich.
  • the size of the effect pigments can have an average value between 5 ⁇ m and 120 ⁇ m, in particular between 10 ⁇ m and 100 ⁇ m, preferably between 30 ⁇ m and 100 ⁇ m. By a relatively exact demarcation of the size of the effect pigments can guarantee ⁇ to that a constant effect effect can be ensured in the application of the powder coating. It can be made the size of the effect pigments, for example, at a defined sample after the initiation of the paint, the Be ⁇ humor. The size is then determined by the equivalent diameter. This diameter can be determined for example by means of appropriate sieves or by microscopic observation and measurement.
  • the size of the effect pigments can be of a standard distribution with egg ⁇ nem mean value and a standard deviation ol less than or equal 50%, in particular less than or equal to 30%, preferably less than or equal to correspond to 10% of the mean.
  • the size distribution of the effect pigments with only a small standard deviation ensures that the desired effect impression on a coated surface is expressed as evenly as possible.
  • the determination of the size distribution of the effect pigments is again carried out on a defined sample after triggering of the paint.
  • the effect pigments can have a breaking edge. Characterized that only a very small proportion of the effect pigments has a breaking edge can be ensured that the effect pigments are not or only slightly damaged and still have their original shape in ⁇ mer. However, it is to be ⁇ into account that a milling step is required in a conventional manufacturing process of powder coating to produce the circuit ⁇ finally to be processed powder coating powder. at It can happen that one or the other effect pigment is damaged in such a grinding process. The fact that only a very small proportion of damaged effect pigments is present, in turn, a uniform appearance effect can be guaranteed.
  • the determination of the proportions of effect pigments with breaking edge preferably takes place at a DEFINE ⁇ th sample after release of the coating.
  • the detection of a breaking edge is preferably carried out by means of light microscopy.
  • the volume fraction of the effect pigments can be between 1% and 50%, in particular between 1% and 30%, preferably between 1% and 10%, of the total volume of the powder coating. By the appropriate proportion of effect pigments can be ensured that a corresponding effect effect is visible in the cured powder coating.
  • the determination of volume fraction can be carried out at a defined sample after release of the coating material as ⁇ derum.
  • the effect pigments can be selected from the list umfas ⁇ send:
  • a layer produced from the powder coating can show a sodium hydroxide resistance of stage 1 after an exposure time of 30 minutes, stage 1 to stage 2 after an exposure time of 60 minutes and stage 1 to stage 3 after an exposure time of 90 minutes and 120 minutes ,
  • the sodium hydroxide resistance is measured as follows:
  • the effect modification for metallics is carried out according to the following rating system according to ISO 4628 Part 1.
  • Test temperature 23 ° C +/- 2 ° C
  • the paint matrix colorant in particular color ⁇ pigments have.
  • the powder coating is colored.
  • Another aspect of the present invention is a powder coating in cured form made from powder coating as previously described.
  • a powder coating has the same properties and features as already described for the powder ⁇ paint in particulate form, in particular in terms of size, size distribution, breaklines, volume fraction and type of effect pigments.
  • Another aspect of the present invention relates to a process for the preparation of powder coating with effect pigments.
  • a homogeneous thermoplastic coating composition of the starting materials in particular comprising binders ⁇ medium, additives, colorants and / or fillers produced.
  • the paint mass is ground after leaving the extruder.
  • the effect pigments are added in an end region of the extruder to ⁇ and homogenized in the viscous coating composition. Due to the fact that the effect pigments are added only in one end region of the extruder, they are only slightly acted upon by the shear forces prevailing in the extruder and are accordingly not or only little damaged.
  • the portion is understood to mean a Endbe ⁇ region of the extruder located close to the outlet opening of the extruder and a protagonistpigmentzudostechnik still possible.
  • the distance between effect pigment metering and the nozzle exit Opening can, measured at the total length of the extruder shaft less than or equal to half, in particular less than or equal to one-third, preferably less than or equal to a quarter of the total length.
  • Extruders are subdivided into a dispersion zone in which components for a thermoplastic powder coating composition are melted and dispersed, and a homogenization zone in which the melted thermoplastic powder coating composition is homogenized.
  • the effect pigments can be added gravimetrically or volumetrically metered. By means of a gravimetric or volumetric addition, it is possible to ensure that precisely the amount of effect pigments which are required for the amount of starting materials processed in the extruder is processed.
  • the effect pigments can be added under protective gas, in particular under nitrogen.
  • the processing under protective gas reduces the risk of explosion, so that a safe, continuous ⁇ ieraji operation can be ensured.
  • the starting materials used in the process may comprise colorants, in particular color pigments.
  • Colored powder coatings with effect pigments are Herge ⁇ over to the ⁇ se.
  • a powder coating according to the invention shows in direct comparison with the customary finished coatings ("dry-blend” powder coating or with means of “bonding” produced powder coating) have a lower separation tendency between the base powder and the effect pigment. As a result, joins the powder application a much more homogeneous deposition virtually no cloud and banding. It goes without saying that in this and the follow ⁇ comparisons identical effect pigments and identi ⁇ rule paint formulations were used.
  • Such a powder coating exhibits a markedly improved recovery stability under standardized application conditions in direct comparison with the customary finished coatings.
  • the inventive powder coating is in the application - even at different high voltages and Triboanassembleen - a significantly higher hue and effect stability in direct ⁇ th compared to the usual refined finishes.
  • the inventive powder coating shows a significantly improved Intelef ⁇ effetbild to the usual refined powder coatings.
  • Classic extrusion of effect pigments is to be understood as meaning that the effect pigments also undergo the dispersion process in the dispersion zone and optionally also a plasticization process upstream of the dispersion process.
  • A3 Separation on the back (with one-sided coating).
  • the effect pigments are incorporated very gently into the coating matrix and the pigment size and pigment distribution are only slightly influenced.
  • the origi ⁇ union pigment sizes are substantially retained. This has a positive influence on the glittering ability (Sparke- lingintenstician) and the graininess (Graininess).
  • the well-knownêttrusion with effect ⁇ pigment offer is already beginning the process section of the extruder where the pigment zesses by traversing the Dispergierpro- be exposed to very high shear stresses and will damage the effect pigments and / or be broken.
  • the powder coatings prepared by the process according to the invention show a significantly increased Sparke- lingintenstician and Graininess.
  • the sparkling intensity of samples can be determined with the aid of the BYK mac i 23 instrument from Altana / Byk.
  • the spar ⁇ klingintenstician returns a measured value on the intensity of the light reflection on the effect pigments in a lacquer layer.
  • the intensities of the samples are measured under 3 different viewing angles (15 °, 45 ° 75 °).
  • the sum of the sparkling intensities can be calculated.
  • the intensity of the sparkling depends on the type of pigment, the proportion of pigment (volume fraction or proportion by weight) in the lacquer layer, the size of the pigment particles and the orientation of the particles.
  • Figure la a micrograph of a sample from a
  • FIG. 1b shows a second micrograph of the sample according to FIG.
  • FIG. 2a a micrograph of a sample of a powder coating according to the invention with effect pigments
  • FIG. 2b shows a second micrograph of the sample according to FIG.
  • FIG. 2a a normal distribution of the size of the effect pigments of an inventive powder coating and a Pul ⁇ verlackes according to the prior art, a schematic representation of an extruder for the production of the inventive powder coating material, a sample for determining the graininess and the Sparkelingintenstician an inventive powder coating layer, a sample for the graininess and the sparkling intensity of a powder coating layer according to the prior art, the direct comparison of the measured graininess of the samples according to FIGS. 5a and 5b, the direct comparison of the measured sparkling intensities of the samples according to FIGS.
  • FIG. 10 shows a sample for determining the separation tendency of effect pigments of a powder coating according to the bonding method
  • FIG. 11 a sample for determining the separation tendency of
  • FIG. 12 shows a sample for evaluating the formation of clouds and streaks in the unannealed state of a powder coating according to the dry-blend method
  • FIG. 13 shows a sample for assessing the clouding and streaking in the uninebrated state of a powder coating according to the bonding method
  • FIG. 14 shows a sample for assessing the formation of clouds and streaks in the unkerbed state of a powder coating according to the method according to the invention
  • FIG. 17a and b a micrograph of powder coating powder according to the method according to the invention in different magnification
  • FIG. 18 a representation of the recovery stability after different times of a powder coating according to the dry-blend method
  • FIG. 19 shows a representation of the recovery stability after different times of a powder coating according to the bonding method
  • FIG. 20 a representation of the recovery stability after different times of a powder coating according to the method according to the invention.
  • Figures la and lb show a first and a second micro ⁇ microscope image of a powder coating from a powder paint with effect pigments 1 according to the prior art, wherein the effect pigments are completely einextrudiert, ie the protagonist ⁇ elements have already been in the initial region of the extruder together with the Supplied starting materials for the preparation of the powder coating.
  • the powder coating layer has a thickness of 60 to 80 ym.
  • the effect pigments 1 are clearly seen as a brilliant par ⁇ Tikel. Striking are the different shape and size of the effect pigments 1. These different shapes are due to the manufacturing process known in the art.
  • the effect pigments are also added simultaneously in the extruder, these are subjected to high shear forces when passing through the extruder and are damaged, for example broken or deformed. Ent ⁇ speaking, the effect pigments 1 no longer exist in its ur ⁇ sprün réelle, usually disk-shaped round shape. In addition, the effective effect size of the effect pigments is reduced.
  • the effect pigments 1 present in FIGS. 1 a and 1 b have a small average size. The smallest of the at ⁇ the figures recognizable effect pigments are only 5 ym and the biggest effect pigments 35 ym large.
  • Figures 2a and 2b are a first and a second micro ⁇ microscope image of a sample of a powder coating from a powder coating according to the invention with effect pigments 1 in the same magnifications as in Figs la and lb shown.
  • the powder coating layer has a thickness of 60 to 80 ym.
  • the effect pigments 1 are again recognizable as shiny particles. It is striking that, in comparison with the figures la and lb, the effect pigments 1 significantly larger and mostly unbeC ⁇ interred visible.
  • FIG. 3 shows a normal distribution of the size of the effect pigments 1 (see Figures 1 and 2) of the inventive powder coating and a powder coating according to the prior art where ⁇ wherein for the latter the effect pigments are completely einextrudiert, ie, the effect pigments have already been in the initial region of the extruder added.
  • the flat curve 4 shows the size distribution of the effect pigments ⁇ of the powder coating according to the prior art
  • currency ⁇ rend the peak curve 5 the size distribution of the effect pigments represents the powder coating according to the invention.
  • the mean size 6 of the flat curve 4 of the effect pigments of the powder coating according to the prior art is significantly smaller than the average size 7 of the effect pigments of the powder coating according to the invention.
  • the standard deviation 8 of the effect pigments of the Pul ⁇ verlackes according to the prior art is significantly greater than the standard deviation of 9 of the effect pigments of the inventive powder coating material.
  • FIG. 4 schematically shows an extruder 10 for producing the powder coating according to the invention.
  • the extruder 10 has an extruder shaft 11 and an extruder head 12.
  • the extruder shaft 11 is driven by a motor 13 via a coupling 14.
  • the individual starting materials which are introduced into the extruder 10 in a hopper 15 at the motor end of the extruder shaft 11, are transported to the extruder head 12.
  • Simultaneously with the transport of the raw materials are mixed this ⁇ 10 with each other in Extru, plasit and homogeneous pergiert discontinuous. Due to the shear forces occurring in the extruder 10, the paint composition is heated from starting materials, which also add ⁇ heat sources are conceivable.
  • the effect pigments are supplied to the extruder 10 through a feed hopper 16 only in the last section of the extruder shaft 11.
  • the extruder shaft 11 can therefore be specially designed in its end region 11 where the effect pigments are supplied, so that the effect pigments are gently incorporated into the paint composition.
  • the extruder shaft illustrated only in the end area 11 has a ⁇ homogenization on which are incorporated the elements bmwpig ⁇ gently into the homogeneous coating matrix.
  • Figures 5a and 5b each show a sample to determine the graininess and the Sparkelingintensmaschine an inventive powder coating layer (5a; A) and a sample of a powder ⁇ lacquer layer according to the prior art by means of conventional
  • FIG. 6 now shows the direct comparison of the measured graininess (Y-axis) of the samples according to FIGS. 5a and 5b (X-axis), whereby the previously described measuring method with the aid of the measuring device BYK maci 23 from Altana / Byk was carried out.
  • the values with the designation A correspond to those of the sample with the powder coating layer according to the invention, while the designation B denotes a powder coating layer after the classical one-pass extrusion.
  • a Grainisess with a value of about 10 for sample B of about 3.5 was determined.
  • FIG. 7 shows the direct comparison of the measured spark-in intensities of the samples (Y-axis) according to FIGS. 5a and 5b. Again, measurements were taken with the BYK mac i 23 measuring instrument from Altana / Byk. Shown are the results of different union among ⁇ viewing angle 10 °, 45 °, 75 ° and the sum ⁇ (X-axis).
  • the Powder coating layer produced by the process according to the invention significantly improved chemical resistance, in particular, for example, against caustic soda in aluminum-containing pigments or gold bronzes.
  • the sodium hydroxide-resistant ⁇ ness corresponds to 30 minutes of the step 1, after 60 min of the step 1, after 90 min, the step 1 and 120 min after the step 1-2 (FIG. 8a).
  • the caustic soda resistance after 30 minutes corresponds to stage 1-2, after 60 minutes stage 2, after 90 minutes stage 3 and after 120 minutes stage 4 (figure 8b).
  • the visual assessment in the caustic soda test (caustic soda resistance) is applied as previously explained in accordance with the Quality Guidelines 631 of the Quality Assurance Association for the general cargo coating of components.
  • FIGS. 9 a and b, 10 a and b and 11 a and b each show a sample for determining the separation tendency of effect pigments of a powder coating according to the dry-blend method (FIG. 9), according to the bonding method (FIG. Fig. 10) and according to the inventive method (Fig. 11).
  • Figure 9b shows the area of the rectangle in Figure 9a in an enlarged view; the same relationship exists for the figures 10 a and 10 b and 11 a and 11 b.
  • Figure 9 a is a very clear Umgriff the powder coating on the back to recognize.
  • the separated effect pigments follow the field lines of the electric field and therefore accumulate concentrated at the edges of the back.
  • the edge of the sheet is remarkably light, which is caused by the delay of Appendices ⁇ separated effect pigments.
  • FIG. 11 a there was no discernible wraparound of the powder coating on the back. There is almost no separation between Ef ⁇ Anlagenffensch and the base powder paint to recognize. In addition, there is no noticeable fluttering of loose effect pigments. This is particularly clear in the enlarged view of an edge of the sheet in Figure 11 b. The edge of the sheet is dark. Thus, no separation of effect pigments from the base powder took place, which could have led to an accumulation of separated effect pigments on the edge.
  • FIGS. 12, 13 and 14 each show a sample for assessing clouding and streaking in the unannoked state of a powder coating according to the dry-blend method (FIG. 12), after the bonding method (FIG. 13) and according to FIG the inventive method ( Figure 14).
  • the powder coating is applied under standardized conditions with the help of the automatic application.
  • the separation of effect pigment and the base powder coating has resulted in strong clouding and banding.
  • Figure 13 only a slight cloud and banding can be seen.
  • no or almost no separation occurs. There are no clouds and no stripes.
  • FIG. 15a and b each show a microscopic photograph of powder coating powder according to the "dry-blend" method at a different magnification, 1500x (FIG. 15a) and 250x (FIG. 15b) - Between the other powder coating particles before.
  • Figures 16a and b is a micrograph of the powder coating powder according to the "bonding" process in different magnifications, 1500x ( Figure 16a) and 250x ( Figure 16b) are shown each. The effect pigments are partially charged with powder ⁇ paint particles.
  • FIGS. 17 a and b each show a microscopic photograph of powder coating powder according to the process of the invention in a different magnification, 1500 ⁇ (FIG. 17 a) and 250 ⁇ (FIG. 17 b).
  • the effect pigments are essentially coated with the paint matrix and therefore difficult to detect.
  • FIGS. 18, 19 and 20 show a representation of the recovery stability after different times (15 min, 30 min, 45 min, 60 min and 75 min) of a powder coating according to the dry-blend method (FIG. 18), according to FIG. bonding "method ( Figure 19) and a powder coating prepared by the method erfindungsgemäs ⁇ sen ( Figure 20).
  • the hue and the effect stability are determined in a standardized recovery test.
  • "Dry-blend" powder coatings already show significant hue and Ef ⁇ Maschinenverschiebungen after a 15 minute exposure in the powder coating cycle.
  • powder coatings prepared stress show a 30 minute in the powder coating cycle clear color tone and effect shifts.
  • powder coatings prepared by the process according to the invention show a significantly higher recovery stability than the two other powder coatings
  • a plant and application parameters are used according to the following table.
  • Test duration 75 minutes Powder output for the circulation ⁇ about 280 grams / minute

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Abstract

A method for producing powder paint having effect pigments, wherein, by means of an extruder (10), a homogeneous thermoplastic paint substance is produced from the starting materials, in particular comprising binders, additives, colorants and/or fillers, and the paint substance is pulverized after it has exited the extruder (10), the effect pigments (1) being added in an end region of the extruder (10) and dispersed in the viscous paint substance.

Description

Pulverlack in partikulärer und ausgehärteter Form mit Effektpigmenten sowie Verfahren zur Herstellung von Pulverlack mit Effektpigmenten Powder coating in particulate and cured form with effect pigments and process for the production of powder coating with effect pigments
Die vorliegende Erfindung betrifft einen Pulverlack in partiku¬ lärer und ausgehärteter Form mit Effektpigmenten sowie Verfahren zur Herstellung von Pulverlack mit Effektpigmenten. The present invention relates to a powder coating in partiku ¬ Lærer and hardened form with effect pigments as well as methods for the preparation of powder paint with effect pigments.
Aus dem Stand der Technik sind verschiedene mit Effektpigmenten versehene Pulverlacke sowie verschiedene Verfahren zu deren Her¬ stellung bekannt. Effektpigmente werden in Pulverlacken zum Erzielen verschiedener optischer Effekte eingesetzt. Dabei stellt sich jeweils die Schwierigkeit, die Effektpigmente gleichmässig im Pulverlack zu verteilen und an oder in den Pulverkörnern nachhaltig zu fixieren, so dass nach der Pulverlackapplikation die ausgehärtete Pulverlackschicht auf dem Substrat ein gleich- mässiges Erscheinungsbild und Funktion gewährleistet. Verschie¬ dene Verfahren zur Veredelung von Pulverlacken mit Effektpigmenten sowie die entsprechenden mit Effektpigmenten versehenen Pulverlacke sind bekannt. Das einfachste Verfahren ist das so ge¬ nannte „dry-blend"-Verfahren, wo eine entsprechende Menge an Ef¬ fektpigmenten dem fertigen Basispulverlack zugefügt wird und in einem Mischvorgang eine homogene Verteilung der Effektpigmente in Basispulverlack erreicht wird. Nachteilig bei diesem Verfahren ist die mangelnde Entmischungsstabilität, welche sich insbe¬ sondere bei der Verarbeitung von grösseren Mengen beispielsweise in automatisierten Pulverlackieranlagen bemerkbar macht. Insbesondere bei einer grösseren beschichteten Fläche kann ein wolkenähnliches Erscheinungsbild entstehen, ausgelöst durch unter¬ schiedliches Auflade- und Abscheideverhalten zwischen den Pulverpartikeln und den trocken zugemischten Effektpigmenten. Weitere Gründe liegen in der unterschiedlichen Dichte zwischen den Pulverlackpartikeln und den Effektpigmenten sowie der unter- schiedlichen Partikelgrösse und Partikelform. Diese mangelnde Entmischungsstabilität macht die entsprechenden Pulverlacke nur bedingt geeignet für die Anwendung in der Architektur beispiels¬ weise zum Beschichten von komplexen geometrischen, effektvollen Fassadenelementen . From the prior art, various provided with effect pigments, powder coatings as well as different processes for their Her ¬ position are known. Effect pigments are used in powder coatings to achieve various optical effects. In each case, there is the difficulty of evenly distributing the effect pigments in the powder coating and of permanently fixing them to or in the powder grains, so that after the powder coating application, the cured powder coating layer on the substrate ensures a uniform appearance and function. Verschie ¬ dene process for refining powder coatings with effect pigments and the corresponding provided with effect pigments powder coatings are known. The simplest method is the so-¬ called "dry-blend" process, where an appropriate amount of Ef ¬ fektpigmenten is added to the final base powder coating and in a mixing process, a homogeneous distribution of the effect pigments is achieved in basic powder coating. A disadvantage of this method is the lack of separation stability, which makes in particular ¬ sondere in the processing of large quantities, for example in automated powder coating noticeable. Particularly in a large coated surface can result in a cloud-like appearance, caused by under ¬ schiedliches charging and deposition behavior between the powder particles and the dry admixed effect pigments, Other reasons include the different density between the powder coating particles and the effect pigments as well as the different particle size and particle shape. This lack of separation stability makes the corresponding powder coatings only conditionally suitable for use in architecture example ¬ example, for coating complex geometric, effective facade elements.
Ein weiteres bekanntes Verfahren ist das so genannte „bonding", wo wiederum die Effektpigmente in einem Batchprozess dem Basis¬ pulverlack zugefügt werden. Im Unterschied zum „dry-blend"- Verfahren wird das Mischen jedoch in einem thermomechanischen Prozess durchgeführt. Durch die in einem Rührprozess erzeugte Reibungswärme wird der Basispulverlack im Mischbehälter aufgeheizt. Dabei ist die Temperatur so zu wählen, dass die einzelnen Partikel des Basispulverlackes bereits weich und klebrig werden, so dass die zu diesem Zeitpunkt zugegebenen Effektpigmente ange¬ bunden werden können. Der so gewonnene Pulverlack ist im Vergleich zu einem mit oben genanntem „dry-blend"-Verfahren gewonnenen Pulverlack deutlich stabiler gegen Entmischung. Nachteilig sind jedoch der aufwändige und nur batchweise durchzuführende Prozess sowie die schwierige Prozesskontrolle. Hierdurch gelingt die Anbindung der Effektpigmente an das Basispulver nur unvollständig. Somit tritt bei der Pulverapplikation wiederum eine Se¬ parierung zwischen Basispulver und nicht angebundenen Effektmittel auf, so dass auch hier, wenn auch weniger ausgeprägt als mit im „dry-blend"-Verfahren hergestelltem Pulverlack, eine streifige oder wolkige Oberfläche nach dem Einbrennen resultieren kann. Another known method is the so-called "bonding", where again the effect pigments are added in a batch process the base ¬ powder coating In contrast to the "dry-blend" -. The method, mixing is, however, carried out in a thermo-mechanical process. The frictional heat generated in a stirring process heats the base powder coating in the mixing vessel. The temperature should be selected so that the individual particles of the powder coating base already be soft and sticky, so that the added at the time effect pigments can be ¬ prevented. The powder coating obtained in this way is significantly more resistant to segregation compared to a powder coating obtained by the above-mentioned "dry-blend" process, but it is disadvantageous to carry out the complex and batch-only process and the difficult process control, thus making it possible to attach the effect pigments to the base powder incomplete. thus, again a Se ¬ are groomed between base powder and unattached effect means occurs during powder application, so that here too, albeit less pronounced than with Created in "dry-blend" process powder coating, a streaky or cloudy surface after Burning can result.
Des Weiteren sind so genannte modifizierte/stabilisierte Effekt¬ pigmente auf dem Markt erhältlich, welche bereits von einer Bin¬ demittelschicht umgeben sind. Diese Effektpigmente allein sind jedoch noch nicht filmbildend. Solche modifizierten Effektpig¬ mente müssen gemäss Herstellerangaben bereits bei der Herstel¬ lung der Pulverlackmischung zugegeben werden und wie die übli- chen Pulverlackzutaten in einem Extruder mittels klassischer Extrusion gleichmässig vermischt und verbunden werden. Nachtei¬ lig an diesem Verfahren ist insbesondere der Umstand, dass die Effektpigmente durch die Verarbeitung im Extruder extremen Furthermore, so-called modified / stabilized effect ¬ pigments on the market which are already surrounded by a bin ¬ demittelschicht. However, these effect pigments alone are not yet film-forming. Such modified Effektpig ¬ elements must be added before the herstel ¬ lung, the powder coating mixture according to manufacturer's instructions and as the usual chen powder coating ingredients are uniformly mixed and connected in an extruder by conventional extrusion. Nachtei ¬ lig of this process is in particular the fact that the effect pigments of extreme by the processing in the extruder
Scherkräften ausgesetzt sind, so dass diese beschädigt und zer¬ teilt werden. Entsprechend müssen mehr Effektpigmente eingesetzt werden, um effektvolle und zufriedenstellende Effekte zu gewähr¬ leisten. Unter Umständen kann sogar das gewünschte Effektbild nicht mit den verfügbaren, stabilisierten Pigmenten erzielt werden . Shear forces are exposed so that they are damaged and zer ¬ shares. Correspondingly more effect pigments must be used to provide effective and satisfactory effects to be granted ¬. Under certain circumstances, even the desired effect image can not be achieved with the available, stabilized pigments.
Es ist Aufgabe der Erfindung, die Nachteile des Standes der Technik zu überwinden. Insbesondere soll einen Pulverlack in partikulärer Form zur Verfügung gestellt werden, welcher sich in der Applikation durch eine hohe Entmischungsstabilität auszeich¬ net . It is an object of the invention to overcome the disadvantages of the prior art. In particular, a powder coating is to be provided in particulate form, which is characterized in the application by a high segregation stability ¬ net.
Schliesslich soll ein Verfahren zur Verfügung gestellt werden, welches ein einfaches und kontrolliertes Herstellen von Pulver¬ lacken mit Effektpigmenten mit einer hohen Gleichmässigkeit erlaubt . Finally, a method is provided which allows a simple and controlled manufacturing of powder paints ¬ with effect pigments having a high regularity.
Diese Aufgabe wird durch die in den unabhängigen Patentansprü¬ chen definierten Vorrichtungen und Verfahren gelöst. Weitere Ausführungsformen ergeben sich aus den abhängigen Patentansprüchen . This object is achieved by the features defined in the independent Patentansprü ¬ chen devices and methods. Further embodiments emerge from the dependent claims.
Ein erfindungsgemässer Pulverlack in partikulärer Form mit Effektpigmenten zeichnet sich dadurch aus, dass die Effektpigmente im Wesentlichen mit einer filmbildenden Lackmatrix benetzt und umhüllt sind. Ein solcher Pulverlack ist zur Filmbildung befähigt. Dabei wird unter „im Wesentlichen mit der Lackmatrix benetzt und umhüllt" verstanden, dass die Oberfläche der Effekt- pigmente wenigstens zu 50%, insbesondere wenigstens zu 75%, be¬ vorzugt wenigstens zu 90% von Lack belegt ist. Durch diese Um¬ hüllung der Effektpigmente mit der Lackmatrix kann gewährleistet werden, dass die umhüllten Effektpigmente bei der elektrostati¬ schen Applikation ein ähnliches Auflade- und Abscheideverhalten aufweisen und sich insofern nur sehr schwer bis gar nicht von den Pulverlackpartikeln entmischen können. Ebenso wird durch die Umhüllung der Effektpigmente mit der Lackmatrix im Lack gewährleistet, dass bei einer späteren Applikation und nachfolgendem Einbrennen des Pulverlackes auf der gesamten Fläche ein gleich- mässiger Effekt erzielt werden kann. Die aus den Pulverlacken gemäss dem Stand der Technik bekannten Wolken- und Streifenbildung wurden so eliminiert. Unter einer Lackmatrix werden die zusammenvermischten Ausgangsstoffe des Pulverlackes ausgenommen der Effektpigmente verstanden. Die zusammenvermischten Ausgangsstoffe des Pulverlackes bilden nach dem Einbrennprozess einen duroplastischen Lackfilm aus. Dementsprechend umfasst eine Lack¬ matrix alle Komponenten, welche für die Ausbildung einer Lackschicht notwendig sind. Die Lackmatrix ist also als identisch zu einem Lack zu verstehen. An inventive powder coating in particulate form with effect pigments is characterized in that the effect pigments are substantially wetted and coated with a film-forming coating matrix. Such a powder coating is capable of film formation. In this context, "wetted and coated essentially with the paint matrix" is understood to mean that the surface of the effect pigments is at least 50%, especially at least 75%, be ¬ vorzugt at least 90% of paint occupied. Through this order ¬ hüllung the effect pigments with the coating matrix can be ensured that the coated effect pigments in elektrostati ¬ rule application have a similar charge and deposition behavior and so far very difficult can not segregate from the powder coating particles up. The coating of the effect pigments with the lacquer matrix in the lacquer likewise ensures that a uniform effect can be achieved over the entire surface during subsequent application and subsequent stoving of the powder lacquer. The known from the powder coatings according to the prior art cloud and banding were eliminated. A paint matrix is understood to mean the mixed-together starting materials of the powder paint except the effect pigments. The mixed-together starting materials of the powder coating form a thermosetting paint film after the baking process. Accordingly, a resist ¬ matrix comprises all components which are necessary for the formation of a lacquer layer. The paint matrix is therefore to be understood as identical to a paint.
Wenigstens 80%, insbesondere wenigstens 90%, bevorzugt wenigs¬ tens 95% aller Effektpigmente können mit der Lackmatrix überzo¬ gen sein. Dieser grosse Anteil an mit Lack überzogenen Effektpigmenten gewährleistet eine einfachere Handhabung des Pulverla¬ ckes . At least 80%, especially at least 90%, preferably Wenig ¬ least 95% of effect pigments can be Plated ¬ gen with the paint matrix. This large amount of paint-coated effect pigments ensures easier handling of the Pulverla ¬ ckes.
Die Bestimmung ob und welcher Anteil der Effektpigmente mit Lack überzogen ist, erfolgt beispielsweise optisch an einer Probe des Pulverlacks. Dabei ist darauf zu achten, dass die Probe derart gross gewählt werden muss, dass eine statistische Aussage mög¬ lich ist. Die Grösse der Effektpigmente kann einen Mittelwert zwischen 5 ym und 120 ym, insbesondere zwischen lOym und 100 ym, bevorzugt zwischen 30 ym und 100 ym liegen. Durch eine relativ genaue Eingrenzung der Grösse der Effektpigmente kann gewährleistet wer¬ den, dass eine gleichbleibende Effektwirkung bei der Auftragung des Pulverlackes gewährleistet werden kann. Dabei kann die Be¬ stimmung der Grösse der Effektpigmente beispielsweise an einer definierten Probe nach dem Auslösen des Lackes erfolgen. Die Grösse wird dann anhand des Äquivalent-Durchmessers bestimmt. Dieser Durchmesser kann beispielsweise mittels entsprechender Siebe oder durch mikroskopische Betrachtung und Messung bestimmt werden . The determination of whether and what proportion of the effect pigments is coated with lacquer is carried out, for example, optically on a sample of the powder lacquer. It is important to ensure that the sample must be so large chosen so that a statistical statement is mög ¬ Lich. The size of the effect pigments can have an average value between 5 μm and 120 μm, in particular between 10 μm and 100 μm, preferably between 30 μm and 100 μm. By a relatively exact demarcation of the size of the effect pigments can guarantee ¬ to that a constant effect effect can be ensured in the application of the powder coating. It can be made the size of the effect pigments, for example, at a defined sample after the initiation of the paint, the Be ¬ humor. The size is then determined by the equivalent diameter. This diameter can be determined for example by means of appropriate sieves or by microscopic observation and measurement.
Die Grösse der Effektpigmente kann einer Normverteilung mit ei¬ nem Mittelwert und einer Standardabweichung ol kleiner oder gleich 50%, insbesondere kleiner oder gleich 30%, bevorzugt kleiner oder gleich 10% des Mittelwerts entsprechen. Durch die Grössenverteilung der Effektpigmente mit einer nur geringen Standardabweichung kann sichergestellt werden, dass der gewünschte Effekteindruck auf einer beschichteten Fläche möglichst gleichmässig zum Ausdruck kommt. Die Bestimmung der Grössenverteilung der Effektpigmente erfolgt wiederum an einer definierten Probe nach Auslösen des Lackes. The size of the effect pigments can be of a standard distribution with egg ¬ nem mean value and a standard deviation ol less than or equal 50%, in particular less than or equal to 30%, preferably less than or equal to correspond to 10% of the mean. The size distribution of the effect pigments with only a small standard deviation ensures that the desired effect impression on a coated surface is expressed as evenly as possible. The determination of the size distribution of the effect pigments is again carried out on a defined sample after triggering of the paint.
Weniger als 40%, insbesondere weniger als 20%, bevorzugt weniger als 10% der Effektpigmente können eine Bruchkante aufweisen. Dadurch, dass nur ein sehr geringer Anteil der Effektpigmente eine Bruchkante aufweist, kann gewährleistet werden, dass die Effektpigmente nicht oder nur wenig beschädigt sind und noch im¬ mer ihre ursprüngliche Form aufweisen. Dabei ist jedoch zu be¬ rücksichtigen, dass bei einem üblichen Herstellungsprozess von Pulverlack ein Schritt des Vermahlens benötigt wird, um schluss¬ endlich das zu verarbeitende Pulverlack-Pulver herzustellen. Bei einem solchen Mahlprozess kann es durchaus vorkommen, dass das eine oder andere Effektpigment beschädigt wird. Dadurch, dass jedoch nur ein sehr geringer Anteil von beschädigten Effektpigmenten vorhanden ist, kann wiederum eine gleichmässige Effekterscheinung gewährleistet werden. Ausserdem wird dadurch gewährleistet, dass der Pulverlack eine ausgezeichnete Witterungs- und Umweltbeständigkeit, insbesondere Lauge- oder Säurebeständig¬ keit, aufweist. Die Bestimmung der Anteile an Effektpigmenten mit Bruchkante erfolgt vorzugsweise wiederum an einer definier¬ ten Probe nach Auslösen des Lackes. Das Erkennen einer Bruchkante wird vorzugsweise mittels Lichtmikroskopie vorgenommen. Less than 40%, in particular less than 20%, preferably less than 10%, of the effect pigments can have a breaking edge. Characterized that only a very small proportion of the effect pigments has a breaking edge can be ensured that the effect pigments are not or only slightly damaged and still have their original shape in ¬ mer. However, it is to be ¬ into account that a milling step is required in a conventional manufacturing process of powder coating to produce the circuit ¬ finally to be processed powder coating powder. at It can happen that one or the other effect pigment is damaged in such a grinding process. The fact that only a very small proportion of damaged effect pigments is present, in turn, a uniform appearance effect can be guaranteed. In addition, this ensures that the powder coating has excellent weathering and environmental resistance, in particular Lauge- or acid resistance ¬ speed. The determination of the proportions of effect pigments with breaking edge preferably takes place at a DEFINE ¬ th sample after release of the coating. The detection of a breaking edge is preferably carried out by means of light microscopy.
Der Volumenanteil der Effektpigmente kann zwischen 1% bis 50%, insbesondere zwischen 1% bis 30%, bevorzugt zwischen 1% und 10% vom Gesamtvolumen des Pulverlackes betragen. Durch den entsprechenden Anteil an Effektpigmenten kann gewährleistet werden, dass eine entsprechende Effektwirkung im ausgehärteten Pulverlack sichtbar wird. Die Bestimmung des Volumenanteils kann wie¬ derum an einer definierten Probe nach Auslösen des Lackes erfolgen . The volume fraction of the effect pigments can be between 1% and 50%, in particular between 1% and 30%, preferably between 1% and 10%, of the total volume of the powder coating. By the appropriate proportion of effect pigments can be ensured that a corresponding effect effect is visible in the cured powder coating. The determination of volume fraction can be carried out at a defined sample after release of the coating material as ¬ derum.
Die Effektpigmente können ausgewählt sein aus der Liste umfas¬ send : The effect pigments can be selected from the list umfas ¬ send:
- Metalleffektpigmente,  - metallic effect pigments,
- Perlglanzpigmente oder Interferenzpigmente,  Pearlescent or interference pigments,
- Leuchtpigmente,  - luminescent pigments,
- Edelstahlpigmente,  - stainless steel pigments,
- Kupferpigmente,  - copper pigments,
- Goldbronzepigmente,  - gold bronze pigments,
- Glasflakes,  - glass flakes,
- Glashohlkugeln,  - glass bubbles,
- Aluminiumpigmente. Eine aus dem Pulverlack hergestellte Schicht kann eine Natron¬ laugenbeständigkeit der Stufe 1 nach einer Einwirkzeit von 30 min, der Stufe 1 bis Stufe 2 nach einer Einwirkzeit von 60 min und der Stufe 1 bis Stufe 3 nach einer Einwirkzeit von 90 min und 120 min zeigen. Dabei wird die Natronlaugenbeständigkeit wie folgt gemessen: - Aluminum pigments. A layer produced from the powder coating can show a sodium hydroxide resistance of stage 1 after an exposure time of 30 minutes, stage 1 to stage 2 after an exposure time of 60 minutes and stage 1 to stage 3 after an exposure time of 90 minutes and 120 minutes , The sodium hydroxide resistance is measured as follows:
Auf die ausgehärtete Pulverlackschicht, wird 24 h nach dem Ein¬ brennen des Lackfilms ein Tropfen einer 10 gew% igen Natronlauge aufgetröpfelt . In Abständen von 30, 60, 90 und 120 min wird die Natronlauge mit einem Weichen, saugfähigen Tuch entfernt und anschliessend die visuelle Veränderung der Oberfläche gem. den Vorgaben und der Vergleichsbilder der GSB-International e.V. bewertet : On the cured powder coating layer, 24 hours after Ein ¬ burn the paint film, a drop of 10 wt% sodium hydroxide solution is dropped. At intervals of 30, 60, 90 and 120 minutes, the caustic soda is removed with a soft, absorbent cloth and then the visual change of the surface acc. the specifications and the comparative images of the GSB International eV rated:
Die visuelle Beurteilung erfolgt gemäss den Qualitätsrichtlinien 631 der Gütegemeinschaft für die Stückgutbeschichtung von Bauteilen (GSB International e.V.) Teil VII, Punkt 25, Ausgabe Mai 2013. The visual assessment is carried out in accordance with the Quality Guidelines 631 of the Gütegemeinschaft für Stückgutbeschichtung von Bauteile (GSB International e.V.) Part VII, Item 25, May 2013 issue.
Die Effektänderung für Metallics wird nach folgendem Bewertungssystem gemäss ISO 4628 Teil 1 durchgeführt.  The effect modification for metallics is carried out according to the following rating system according to ISO 4628 Part 1.
Stufe 1 Kein Unterschied zwischen der getesteten Oberfläche und der Vorlage (nichtgetestete Oberfläche) Level 1 No difference between the tested surface and the original (untested surface)
Stufe 2 Kaum sichtbare Färb- und Effektveränderungen Level 2 Barely visible color and effect changes
Stufe 3 Sichtbare Färb- und Effektveränderungen Level 3 Visible color and effect changes
Stufe 4 Deutliche sichtbare Färb- und Effektveränderungen Level 4 Clear visible color and effect changes
Stufe 5 Markante Farbveränderungen - vollständiger Effektverlust Level 5 Striking color changes - complete loss of effect
Vorgaben : Requirements :
Konzentration der Natronlauge: 10 Gew % = ca. 2,5 N  Concentration of the sodium hydroxide solution: 10% by weight = approx. 2.5 N
Prüftemperatur : 23 °C +/- 2°C Test temperature: 23 ° C +/- 2 ° C
Dauer der Belastung: 30, 60, 90, 120 min Beurteilung : visuelle Beurteilung gem. den Duration of load: 30, 60, 90, 120 min Assessment: visual assessment acc. the
Qualitätsrichtlinien RL-631 der Gütegemeinschaft für die Stück- gutbeschichtung von Bauteilen (GSB International e.V.) Teil VII, Punkt 25, Ausgabe Mai 2013  Quality Guidelines RL-631 of the Quality Assurance Association for the Particle Coating of Components (GSB International e.V.) Part VII, Item 25, May 2013 issue
Des Weiteren kann die Lackmatrix Farbmittel, insbesondere Farb¬ pigmente, aufweisen. Auf diese Weise ist der Pulverlack gefärbt. Furthermore, the paint matrix colorant, in particular color ¬ pigments have. In this way, the powder coating is colored.
Ein weiterer Aspekt der vorliegenden Erfindung ist ein Pulverlack in ausgehärteter Form hergestellt aus Pulverlack wie vorgängig beschrieben. Dabei weist ein solcher Pulverlack dieselben Eigenschaften und Merkmale auf, wie sie bereits für den Pulver¬ lack in partikulärer Form beschrieben sind, insbesondere hinsichtlich Grösse, Grössenverteilung, Bruchkanten, Volumenanteil und Art der Effektpigmente. Another aspect of the present invention is a powder coating in cured form made from powder coating as previously described. In this case, such a powder coating has the same properties and features as already described for the powder ¬ paint in particulate form, in particular in terms of size, size distribution, breaklines, volume fraction and type of effect pigments.
Ein weiterer Aspekt der vorliegenden Erfindung betrifft ein Verfahren zur Herstellung von Pulverlack mit Effektpigmenten. Dabei wird mittels eines Extruders eine homogene thermoplastische Lackmasse aus den Ausgangsstoffen, insbesondere umfassend Binde¬ mittel, Additive, Farbmittel und/oder Füllstoffe, hergestellt. Die Lackmasse wird nach dem Verlassen des Extruders vermählen. Die Effektpigmente werden in einem Endbereich des Extruders zu¬ gegeben und in der viskosen Lackmasse homogenisiert. Dadurch, dass die Effektpigmente erst in einem Endbereich des Extruders zugegeben werden, werden diese nur noch geringfügig durch die im Extruder herrschenden Scherkräfte beaufschlagt und entsprechend nicht oder nur wenig beschädigt. Dabei wird unter einem Endbe¬ reich des Extruders derjenige Bereich verstanden, welcher sich in unmittelbarer Nähe zur Austrittsöffnung des Extruders befindet und eine Effektpigmentzudosierung noch ermöglicht. Der Abstand zwischen Effektpigmentzudosierung und der Düsenaustritts- Öffnung kann, gemessen an der Gesamtlänge der Extruderwelle kleiner oder gleich der Hälfte, insbesondere kleiner oder gleich einem Drittel, bevorzugt kleiner oder gleich einem Viertel der Gesamtlänge betragen. Extruder werden in eine Dispergierungszo- ne, in welcher Komponenten für eine thermoplastische Pulverlackmasse aufgeschmolzen und dispergiert werden, und einer Homo- geniserungszone, in welcher die aufgeschmolzene thermoplastische Pulverlackmasse homogenisert wird, unterteilt. Die Effektpig¬ mentzudosierung findet entsprechend in der Homogenisierungszone des Extruders statt, wo der Dispergierprozess der geschmolzenen Pulverlackmasse vollständig abgeschlossen ist. Dies hat zur Fol¬ ge, dass die zudosierten Effektpigmente ausschliesslich dem Ho- mogenisierungsprozess in der Homogenisierungszone unterzogen werden . Another aspect of the present invention relates to a process for the preparation of powder coating with effect pigments. In this case, by means of an extruder, a homogeneous thermoplastic coating composition of the starting materials, in particular comprising binders ¬ medium, additives, colorants and / or fillers produced. The paint mass is ground after leaving the extruder. The effect pigments are added in an end region of the extruder to ¬ and homogenized in the viscous coating composition. Due to the fact that the effect pigments are added only in one end region of the extruder, they are only slightly acted upon by the shear forces prevailing in the extruder and are accordingly not or only little damaged. In this case, the portion is understood to mean a Endbe ¬ region of the extruder located close to the outlet opening of the extruder and a Effektpigmentzudosierung still possible. The distance between effect pigment metering and the nozzle exit Opening can, measured at the total length of the extruder shaft less than or equal to half, in particular less than or equal to one-third, preferably less than or equal to a quarter of the total length. Extruders are subdivided into a dispersion zone in which components for a thermoplastic powder coating composition are melted and dispersed, and a homogenization zone in which the melted thermoplastic powder coating composition is homogenized. The Effektpig ¬ mentzudosierung takes place according to the homogenization of the extruder where the dispersing of the molten powder coating composition is complete. This has to be subjected to Fol ¬ ge that the metered effect pigments exclusively mogenisierungsprozess the Ho in the homogenization.
Die Effektpigmente können gravimetrisch oder volumetrisch dosiert zugegeben werden. Durch eine gravimetrische oder volumet- rische Zugabe kann gewährleistet werden, dass genau diejenige Menge an Effektpigmenten verarbeitet wird, welche zu der im Extruder verarbeiteten Menge an Ausgangsstoffen benötigt werden. The effect pigments can be added gravimetrically or volumetrically metered. By means of a gravimetric or volumetric addition, it is possible to ensure that precisely the amount of effect pigments which are required for the amount of starting materials processed in the extruder is processed.
Die Effektpigmente können unter Schutzgas, insbesondere unter Stickstoff, zugegeben werden. Die Verarbeitung unter Schutzgas reduziert das Explosionsrisiko, so dass ein sicherer, kontinu¬ ierlicher Betrieb gewährleistet werden kann. The effect pigments can be added under protective gas, in particular under nitrogen. The processing under protective gas reduces the risk of explosion, so that a safe, continuous ¬ ierlicher operation can be ensured.
Des Weiteren können die in dem Verfahren eingesetzten Ausgangsstoffe Farbmittel, insbesondere Farbpigmente, umfassen. Auf die¬ se Weise werden gefärbte Pulverlacke mit Effektpigmenten herge¬ stellt. Furthermore, the starting materials used in the process may comprise colorants, in particular color pigments. Colored powder coatings with effect pigments are Herge ¬ over to the ¬ se.
Ein erfindungsgemässer Pulverlack zeigt im direkten Vergleich zu den üblichen veredelten Lacken („dry-blend"-Pulverlack oder mit- tels „bonding" hergestellter Pulverlack) eine geringere Separationsneigung zwischen dem Grundpulver und dem Effektpigment. Infolge dessen tritt bei der Pulverapplikation eine deutlich homogenere Abscheidung nahezu ohne Wolken- und Streifenbildung auf. Es versteht sich von selbst, dass bei diesem und den nachfolgen¬ den Vergleichen jeweils identische Effektpigmente und identi¬ schen Lackrezepturen verwendet wurden. A powder coating according to the invention shows in direct comparison with the customary finished coatings ("dry-blend" powder coating or with means of "bonding" produced powder coating) have a lower separation tendency between the base powder and the effect pigment. As a result, joins the powder application a much more homogeneous deposition virtually no cloud and banding. It goes without saying that in this and the follow ¬ comparisons identical effect pigments and identi ¬ rule paint formulations were used.
Ein solcher Pulverlack zeigt unter standardisierten Applikationsbedingungen im direkten Vergleich zu den üblichen veredelten Lacken eine deutliche verbesserte Rückgewinnungsstabilität. Such a powder coating exhibits a markedly improved recovery stability under standardized application conditions in direct comparison with the customary finished coatings.
Der erfindungsgemässe Pulverlack zeigt bei der Applikation - auch bei unterschiedlichen Hochspannungen und Triboanwendungen - eine signifikant höhere Farbton- und Effektstabilität im direk¬ ten Vergleich zu den üblichen veredelten Lacken. The inventive powder coating is in the application - even at different high voltages and Triboanwendungen - a significantly higher hue and effect stability in direct ¬ th compared to the usual refined finishes.
Der erfindungsgemässe Pulverlack zeigt gegenüber den üblichen veredelten Pulverlacken ein signifikant verbessertes Gesamtef¬ fektbild. Im direkten Vergleich von Pulverlackproben aus erfin- dungsgemässem Pulverlack zu Pulverlacken, welche durch klassische Einextrusion von Effektpigmenten in die Pulverlackmatrix bei gleicher GesamtZusammensetzung hergestellt wurden, zeigen die erfindungsgemässen Pulverlacke in den nachfolgend aufgezeig¬ ten Bewertungskriterien AI, A2, A3 bei allen Punkten Benotungen von <= 2. Unter klassischer Einextrusion von Effepktpigmenten ist zu verstehen, dass die Effektpigmente auch den Dispergie- rungsprozess in der Dispergierungszone und gegebenenfalls auch einen dem Dispergierungprozess vorgelagerten Plastifizierungs- prozess durchlaufen. Unter dem Plastifizierungsprozess wird all¬ gemein das Aufschmelzen einer Pulverlackvormischung verstanden und unter dem Dispergierungsprozess ein Zerreiben/Zerteilung der vorliegenden Pigment- und Füllstoffagglomerate . Die Beurteilung des Effektbildes von applizierten und einge¬ brannten Pulverlacken erfolgt visuell im direkten Vergleich der Proben : The inventive powder coating shows a significantly improved Gesamtef ¬ fektbild to the usual refined powder coatings. In a direct comparison of powder paint samples from inventions dungsgemässem powder coating to powder coatings which have been produced by classical Einextrusion of effect pigments in the powder coating matrix with the same overall composition, the novel powder coatings show in the following be displayed ¬ th evaluation criteria AI, A2, A3 at all points evaluations of < = 2. Classic extrusion of effect pigments is to be understood as meaning that the effect pigments also undergo the dispersion process in the dispersion zone and optionally also a plasticization process upstream of the dispersion process. Under the plasticizing process, the melting of a Pulverlackvormischung is meant all ¬ mean and under the dispersion process, a grinding / dicing of the present pigment and filler agglomerates. The assessment of the effect image of applied and been burned ¬ powder coatings visually direct comparison of samples:
Kriterien für die Beurteilung der Homogenität der Effektverteilung der beschichteten und eingebrannten Pulverlacke: Criteria for assessing the homogeneity of the effect distribution of the coated and baked powder coatings:
AI: Effektverteilung auf der Fläche (Streifen & Wolken) AI: Effect distribution on the surface (stripes & clouds)
A2 : Effektanhäufung / -Verarmung auf den Kanten A2: Effect accumulation / depletion on the edges
A3: Separierung auf der Rückseite (bei einseitiger Beschich- tung) . A3: Separation on the back (with one-sided coating).
Bedeutung der Bewertungsziffern: Meaning of the evaluation numbers:
1 - deutlich besser/höher/grösser als die Vergleichsprobe 1 - significantly better / higher / greater than the comparative sample
2 - besser/höher/grösser als die Vergleichsprobe  2 - better / higher / greater than the comparative sample
3 - Vergleichbar mit der Vergleichsprobe  3 - Comparable to the comparative sample
4 - schlechter/niedriger/kleiner als die Vergleichsprobe  4 - worse / lower / smaller than the comparative sample
5 - deutlich schlechter/niedriger/kleiner als die Vergleichsprobe  5 - significantly worse / lower / smaller than the comparative sample
Mit dem vorgängig geschilderten erfindungsgemässen Verfahren zur Herstellung von Pulverlacken werden die Effektpigmente äusserst schonend in die Lackmatrix eingearbeitet und die Pigmentgrösse und Pigmentverteilung nur geringfügig beeinflusst. Die ursprüng¬ lichen Pigmentgrössen bleiben im Wesentlichen erhalten. Dieses hat einen positiven Einfluss auf die Glitzerfähigkeit (Sparke- lingintensität ) und die Körnigkeit (Graininess) . Im Gegensatz hierzu steht die bekannte Einextrusion mit Effekt¬ pigmentzugabe bereits zu Begin der Prozessstrecke des Extruders, wo die Pigmentteilchen durch das Durchlaufen des Dispergierpro- zesses sehr starken Scherbeanspruchungen ausgesetzt werden und die Effektpigmente dabei beschädigt und/oder zerteilt werden. With the previously described process according to the invention for the production of powder coatings, the effect pigments are incorporated very gently into the coating matrix and the pigment size and pigment distribution are only slightly influenced. The origi ¬ union pigment sizes are substantially retained. This has a positive influence on the glittering ability (Sparke- lingintensität) and the graininess (Graininess). In contrast, the well-known Einextrusion with effect ¬ pigment encore is already beginning the process section of the extruder where the pigment zesses by traversing the Dispergierpro- be exposed to very high shear stresses and will damage the effect pigments and / or be broken.
Im direkten Vergleich von Proben ausgehend von der gleichen Pigmenttype, derselben Pigmentgrössenverteilung, und einer identischen Lackmatrix zeigen die nach dem erfindungsgemässen Verfahren hergestellten Pulverlacke eine signifikant erhöhte Sparke- lingintensität und Graininess. In a direct comparison of samples starting from the same pigment type, the same pigment size distribution, and an identical coating matrix, the powder coatings prepared by the process according to the invention show a significantly increased Sparke- lingintensität and Graininess.
Die Sparkelingintensität von Proben kann mit Hilfe des Gerätes BYK mac i 23 von der Fa. Altana /Byk bestimmt werden. Die Spar¬ klingintensität gibt einen Messwert wieder über die Intensität der Lichtreflexion an den Effektpigmenten in einer Lackschicht. Die Intensitäten der Proben werden dabei unter 3 verschiedenen Betrachungswinkeln vermessen (15°, 45° 75°). Zusätzlich kann die Summe der Sparklingintensitäten berechnet werden. The sparkling intensity of samples can be determined with the aid of the BYK mac i 23 instrument from Altana / Byk. The spar ¬ klingintensität returns a measured value on the intensity of the light reflection on the effect pigments in a lacquer layer. The intensities of the samples are measured under 3 different viewing angles (15 °, 45 ° 75 °). In addition, the sum of the sparkling intensities can be calculated.
Die Sparklingintensität ist dabei abhängig von der Pigmenttype, vom Pigmentanteil (Volumenanteil oder Gewichtsanteil) in der Lackschicht, der Grösse der Pigmentteilchen und der Orientierung der Teilchen. The intensity of the sparkling depends on the type of pigment, the proportion of pigment (volume fraction or proportion by weight) in the lacquer layer, the size of the pigment particles and the orientation of the particles.
Je grösser dieser Wert ist, desto stärker ist die Lichtreflexion und umso effektvoller erscheint die Lackschicht. The greater this value, the stronger the light reflection and the more effective the varnish layer appears.
Die Sparkelingintensität des neuen Pulverlackes / Pulverlack¬ films liegt dabei je nach Betrachtungswinkel signifikant >= 30% insbesondere >= 65% bevorzugt >= 100 % höher im Vergleich zu der klassischen Einextrusion von Effektpigmenten. Die Graininess (Körnigkeit) von Proben kann dabei mit Hilfe des Gerätes BYK mac i 23 von der Fa. Altana /Byk bestimmt werden. Der Wert der Graininess beschreibt bei diffuser Beleuchtung das Vorhandensein von hell-dunkel Flächen und liefert somit quanti¬ tative Aussagen hierzu. Die Graininess wird beeinflusst durch die Pigmentart, die Pigmentgrösse und Grössenverteilung, die Pigmentorientierung und die Pigmentverteilung. Die Werte liegen dabei im Bereich von Graininess G = 0 (keine hell-dunkel Flä¬ chen) bis zu G = 15 (maximale Verteilung von hell-dunkel Flä¬ chen) . The Sparkelingintensität of the new powder paint / powder coating ¬ film is, depending on the viewing angle significant> = 30%, in particular> = 65%, preferably> = 100% higher compared to the classical Einextrusion of effect pigments. The graininess (granularity) of samples can be determined using the BYK mac i 23 device from Altana / Byk. The value of the graininess describes in diffuse light, the presence of light and dark areas and thus provides quanti ¬ tative statements for this purpose. Graininess is influenced by the type of pigment, the pigment size and size distribution, the pigment orientation and the pigment distribution. The values are in the range of graininess G = 0 (no light-dark FLAE ¬ chen) to G = 15 (maximum distribution of light-dark FLAE ¬ chen).
Die Graininess des neuen Pulverlackfilms kann dabei signifikant >= 30%, insbesondere >= 65%, bevorzugt >= 100 %, höher liegen im Vergleich zu der klassischen Einextrusion von Effektpigmenten. The graininess of the new powder coating film can be significantly> = 30%, in particular> = 65%, preferably> = 100%, higher in comparison to the classical one-pass extrusion of effect pigments.
Anhand von Figuren, welche lediglich Ausführungsbeispiele dar¬ stellen, wird die Erfindung im Folgenden näher erläutert. Es zeigen : On the basis of figures, which represent only exemplary embodiments ¬ , the invention will be explained in more detail below. Show it :
Figur la: eine mikroskopische Aufnahme einer Probe aus einem Figure la: a micrograph of a sample from a
Pulverlack mit Effektpigmenten nach dem Stand der Technik,  Powder coating with effect pigments according to the prior art,
Figur lb: eine zweite mikroskopische Aufnahme der Probe nach FIG. 1b shows a second micrograph of the sample according to FIG
Figur la,  Figure la,
Figur 2a: eine mikroskopische Aufnahme einer Probe aus einem erfindungsgemässen Pulverlack mit Effektpigmenten, FIG. 2a: a micrograph of a sample of a powder coating according to the invention with effect pigments,
Figur 2b: eine zweite mikroskopische Aufnahme der Probe nach FIG. 2b shows a second micrograph of the sample according to FIG
Figur 2a, eine Normalverteilung der Grösse der Effektpigmente eines erfindungsgemässen Pulverlackes und eines Pul¬ verlackes nach dem Stand der Technik, eine schematische Darstellung eines Extruders zur Herstellung des erfindungsgemässen Pulverlackes, eine Probe zur Bestimmung der Graininess und der Sparkelingintensität einer erfindungsgemässen Pulverlackschicht, eine Probe zur Bestimmung der Graininess und der Sparkelingintensität einer Pulverlackschicht nach dem Stand der Technik, der direkte Vergleich der gemessenen Graininess der Proben gemäss den Figuren 5a und 5b, der direkte Vergleich der gemessenen Sparkelinginten- sitäten der Proben gemäss den Figuren 5a und 5b, eine Probe zur Bestimmung der Natronlaugenbeständig¬ keit einer erfindungsgemässen Pulverlackschicht, eine Probe zur Bestimmung der Natronlaugenbeständig¬ keit einer Pulverlackschicht nach dem Stand der Tech¬ nik, eine Probe zur Bestimmung der Separationsneigung von Effektpigmenten eines Pulverlackes nach dem „dry- blend"-Verfahren, Figur 10: eine Probe zur Bestimmung der Separationsneigung von Effektpigmenten eines Pulverlackes nach dem „bonding"-Verfahren, FIG. 2a, a normal distribution of the size of the effect pigments of an inventive powder coating and a Pul ¬ verlackes according to the prior art, a schematic representation of an extruder for the production of the inventive powder coating material, a sample for determining the graininess and the Sparkelingintensität an inventive powder coating layer, a sample for the graininess and the sparkling intensity of a powder coating layer according to the prior art, the direct comparison of the measured graininess of the samples according to FIGS. 5a and 5b, the direct comparison of the measured sparkling intensities of the samples according to FIGS. 5a and 5b, a sample for determining the caustic soda resistant ness of an inventive powder coating layer, a sample to determine the sodium hydroxide-resistant ¬ ness of a powder coating according to the prior Tech ¬ technology, a sample for determining the separation tendency of effect pigments of a powder coating according to the "Dry-blend" process, FIG. 10 shows a sample for determining the separation tendency of effect pigments of a powder coating according to the bonding method;
Figur 11: eine Probe zur Bestimmung der Separationsneigung von FIG. 11: a sample for determining the separation tendency of
Effektpigmenten eines Pulverlackes nach dem erfin- dungsgemässen Verfahren,  Effect pigments of a powder coating according to the process of the invention,
Figur 12: eine Probe zur Beurteilung der Wolken- und Streifenbildung im uneingebrannten Zustand eines Pulverlackes nach dem „dry-blend"-Verfahren, FIG. 12 shows a sample for evaluating the formation of clouds and streaks in the unannealed state of a powder coating according to the dry-blend method,
Figur 13: eine Probe zur Beurteilung der Wolken- und Streifenbildung im uneingebrannten Zustand eines Pulverlackes nach dem „bonding"-Verfahren, FIG. 13 shows a sample for assessing the clouding and streaking in the uninebrated state of a powder coating according to the bonding method;
Figur 14: eine Probe zur Beurteilung der Wolken- und Streifenbildung im uneingebrannten Zustand eines Pulverlackes nach dem erfindungsgemässen Verfahren, FIG. 14 shows a sample for assessing the formation of clouds and streaks in the unkerbed state of a powder coating according to the method according to the invention;
Figur 15a und b: eine mikroskopische Aufnahme von Pulverlack- Pulver nach dem „dry-blend"-Verfahren in unterschiedlicher Vergrösserung, 15a and b: a micrograph of powder coating powder according to the "dry-blend" method in different magnification,
Figur 16a und b: eine mikroskopische Aufnahme von Pulverlack- Pulver nach dem „bonding"-Verfahren in unterschiedlicher Vergrösserung, 16a and b: a micrograph of powder coating powder according to the "bonding" method in different magnification,
Figur 17a und b: eine mikroskopische Aufnahme von Pulverlack- Pulver nach dem erfindungsgemässen Verfahren in unterschiedlicher Vergrösserung, Figur 18: eine Darstellung der Rückgewinnungsstabilität nach unterschiedlichen Zeiten eines Pulverlackes nach dem „dry-blend"-Verfahren, 17a and b: a micrograph of powder coating powder according to the method according to the invention in different magnification, FIG. 18: a representation of the recovery stability after different times of a powder coating according to the dry-blend method,
Figur 19: eine Darstellung der Rückgewinnungsstabilität nach unterschiedlichen Zeiten eines Pulverlackes nach dem „bonding"-Verfahren, und FIG. 19 shows a representation of the recovery stability after different times of a powder coating according to the bonding method, and FIG
Figur 20: eine Darstellung der Rückgewinnungsstabilität nach unterschiedlichen Zeiten eines Pulverlackes nach dem erfindungsgemässen Verfahren. FIG. 20: a representation of the recovery stability after different times of a powder coating according to the method according to the invention.
Die Figuren la und lb zeigen eine erste und eine zweite mikro¬ skopische Aufnahme einer Pulverlackschicht aus einem Pulverlack mit Effektpigmenten 1 nach dem Stand der Technik, wobei die Effektpigmente vollständig einextrudiert sind, d.h. die Effektpig¬ mente wurden bereits im Anfangsbereich des Extruders zusammen mit den Ausgangsstoffen zur Herstellung des Pulverlackes beigegeben. Die Pulverlackschicht weist eine Dicke von 60 bis 80 ym auf. Die Effektpigmente 1 sind dabei deutlich als glänzende Par¬ tikel zu erkennen. Auffallend sind die unterschiedliche Form und Grösse der Effektpigmente 1. Diese unterschiedlichen Formen sind durch den im Stand der Technik bekannten Herstellungsprozess bedingt. Wenn beim Vermischen und Dispergieren der für den Pulverlack benötigten Ausgangsstoffe die Effektpigmente ebenfalls gleichzeitig im Extruder beigegeben werden, sind diese beim Durchlaufen durch den Extruder hohen Scherkräften ausgesetzt und werden beschädigt, beispielsweise gebrochen oder verformt. Ent¬ sprechend liegen die Effektpigmente 1 nicht mehr in ihrer ur¬ sprünglichen, meist scheibenförmig runden Form vor. Ausserdem wird die für die Effektwirkung wirksame Grösse der Effektpigmente reduziert. Die in den Figuren la und lb vorliegenden Effektpigmente 1 wei¬ sen ein geringe mittlere Grösse auf. Die kleinsten auf den bei¬ den Abbildungen zu erkennenden Effektpigmente sind lediglich 5 ym und die grössten Effektpigmente 35 ym gross. Figures la and lb show a first and a second micro ¬ microscope image of a powder coating from a powder paint with effect pigments 1 according to the prior art, wherein the effect pigments are completely einextrudiert, ie the Effektpig ¬ elements have already been in the initial region of the extruder together with the Supplied starting materials for the preparation of the powder coating. The powder coating layer has a thickness of 60 to 80 ym. The effect pigments 1 are clearly seen as a brilliant par ¬ Tikel. Striking are the different shape and size of the effect pigments 1. These different shapes are due to the manufacturing process known in the art. If, during mixing and dispersion of the starting materials required for the powder coating, the effect pigments are also added simultaneously in the extruder, these are subjected to high shear forces when passing through the extruder and are damaged, for example broken or deformed. Ent ¬ speaking, the effect pigments 1 no longer exist in its ur ¬ sprünglichen, usually disk-shaped round shape. In addition, the effective effect size of the effect pigments is reduced. The effect pigments 1 present in FIGS. 1 a and 1 b have a small average size. The smallest of the at ¬ the figures recognizable effect pigments are only 5 ym and the biggest effect pigments 35 ym large.
In den Figuren 2a und 2b sind eine erste und eine zweite mikro¬ skopische Aufnahme einer Probe einer Pulverlackschicht aus einem erfindungsgemässen Pulverlack mit Effektpigmenten 1 in den gleichen Vergrösserungen wie in den Figuren la bzw. lb dargestellt. Die Pulverlackschicht weist eine Dicke von 60 bis 80 ym auf. Die Effektpigmente 1 sind wiederum als glänzende Partikel erkennbar. Auffallend ist, dass im Vergleich zu den Figuren la und lb die Effektpigmente 1 signifikant grösser und mehrheitlich unbeschä¬ digt zu erkennen sind. Die für die Herstellung des Pulverlackes verwendeten Effektpigmente waren für beide Proben gemäss den Figuren 1 und den Figuren 2 gleich gross ( Di o= 26-30 ym, D5 o= 63-71 ym, D90= 100-108 ym) . Es zeigt sich jedoch, dass durch ein scho¬ nenderes Einbringen der Effektpigmente in den Pulverlack die Effektpigmente nur geringfügig beschädigt wurden und entsprechend grösser sind. In Figures 2a and 2b are a first and a second micro ¬ microscope image of a sample of a powder coating from a powder coating according to the invention with effect pigments 1 in the same magnifications as in Figs la and lb shown. The powder coating layer has a thickness of 60 to 80 ym. The effect pigments 1 are again recognizable as shiny particles. It is striking that, in comparison with the figures la and lb, the effect pigments 1 significantly larger and mostly unbeschä ¬ interred visible. The effect pigments used for the preparation of the powder coating were the same for both samples according to FIGS. 1 and 2 (Di o = 26-30 ym, D 5 o = 63-71 ym, D 90 = 100-108 ym). It is found, however, that the effect pigments are only slightly damaged by scho ¬ nenderes introduction of the effect pigments in the powder paint and are correspondingly greater.
Die Figur 3 zeigt eine Normalverteilung der Grösse der Effektpigmente 1 (siehe Figuren 1 und 2) eines erfindungsgemässen Pulverlackes und eines Pulverlackes nach dem Stand der Technik, wo¬ bei für letzteres die Effektpigmente vollständig einextrudiert sind, d.h. die Effektpigmente wurden bereits im Anfangsbereich des Extruders beigegeben. Die für die Herstellung der Pulverlacke (erfindungsgemässer Pulverlack und Pulverlack nach dem Stand der Technik) verwendeten Effektpigmente waren für beide Pulverlacke gleich gross ( Di o= 26-30 ym, D50= 63-71 ym, D90= 100-108 ym) . Die flache Kurve 4 stellt die Grössenverteilung der Effekt¬ pigmente des Pulverlackes nach dem Stand der Technik dar, wäh¬ rend die spitze Kurve 5 die Grössenverteilung der Effektpigmente des erfindungsgemässen Pulverlackes darstellt. Die mittlere Grösse 6 der flachen Kurve 4 der Effektpigmente des Pulverlackes nach dem Stand der Technik ist deutlich kleiner als die mittlere Grösse 7 der Effektpigmente des erfindungsgemässen Pulverlackes. Ebenso ist die Standardabweichung 8 der Effektpigmente des Pul¬ verlackes nach dem Stand der Technik deutlich grösser als die Standardabweichung 9 der Effektpigmente des erfindungsgemässen Pulverlackes . 3 shows a normal distribution of the size of the effect pigments 1 (see Figures 1 and 2) of the inventive powder coating and a powder coating according to the prior art where ¬ wherein for the latter the effect pigments are completely einextrudiert, ie, the effect pigments have already been in the initial region of the extruder added. The effect pigments used for the preparation of the powder coatings (inventive powder coating and powder coating according to the prior art) were the same size for both powder coatings (Di o = 26-30 ym, D 50 = 63-71 ym, D 90 = 100-108 ym) , The flat curve 4 shows the size distribution of the effect pigments ¬ of the powder coating according to the prior art, currency ¬ rend the peak curve 5, the size distribution of the effect pigments represents the powder coating according to the invention. The mean size 6 of the flat curve 4 of the effect pigments of the powder coating according to the prior art is significantly smaller than the average size 7 of the effect pigments of the powder coating according to the invention. Also, the standard deviation 8 of the effect pigments of the Pul ¬ verlackes according to the prior art is significantly greater than the standard deviation of 9 of the effect pigments of the inventive powder coating material.
In der Figur 4 ist schematisch ein Extruder 10 zur Herstellung des erfindungsgemässen Pulverlackes dargestellt. Der Extruder 10 weist eine Extruderwelle 11 und einen Extruderkopf 12 auf. Die Extruderwelle 11 wird über eine Kupplung 14 von einem Motor 13 angetrieben. Durch die Drehbewegung der Extruderwelle werden die einzelnen Ausgangsstoffe, welche in einem Einfülltrichter 15 an motorseitigen Ende der Extruderwelle 11 in den Extruder 10 eingefüllt werden, zum Extruderkopf 12 transportiert. Gleichzeitig mit dem Transportieren der Ausgangsstoffe werden diese im Extru¬ der 10 untereinander vermischt, plasitifiziert und homogen dis- pergiert. Durch die im Extruder 10 auftretenden Scherkräfte wird die Lackmasse aus Ausgangsstoffen erwärmt, wobei auch zusätzli¬ che Wärmequellen denkbar sind. Erfindungsgemäss werden die Effektpigmente erst im letzten Abschnitt der Extruderwelle 11 dem Extruder 10 durch einen Einfülltrichter 16 zugeführt. Die Extruderwelle 11 kann in ihrem Endbereich 11 also dort wo die Effektpigmente zugeführt werden, speziell ausgestaltet sein, so dass die Effektpigmente schonend in die Lackmasse eingearbeitet werden. Die dargestellte Extruderwelle weist im Endbereich 11 λ nur noch einen Homogenisierungszone auf, welche die Effektpig¬ mente schonend in die homogene Lackmatrix einarbeitet. Es sind ebenfalls Extruder mit mehreren Extruderwellen denkbar. Die Figuren 5a und 5b zeigen je eine Probe zur Bestimmung der Graininess und der Sparkelingintensität einer erfindungsgemässen Pulverlackschicht (Figur 5a; A) und einer Probe einer Pulver¬ lackschicht nach dem Stand der Technik mittels klassischer FIG. 4 schematically shows an extruder 10 for producing the powder coating according to the invention. The extruder 10 has an extruder shaft 11 and an extruder head 12. The extruder shaft 11 is driven by a motor 13 via a coupling 14. As a result of the rotational movement of the extruder shaft, the individual starting materials, which are introduced into the extruder 10 in a hopper 15 at the motor end of the extruder shaft 11, are transported to the extruder head 12. Simultaneously with the transport of the raw materials are mixed this ¬ 10 with each other in Extru, plasitifiziert and homogeneous pergiert discontinuous. Due to the shear forces occurring in the extruder 10, the paint composition is heated from starting materials, which also add ¬ heat sources are conceivable. According to the invention, the effect pigments are supplied to the extruder 10 through a feed hopper 16 only in the last section of the extruder shaft 11. The extruder shaft 11 can therefore be specially designed in its end region 11 where the effect pigments are supplied, so that the effect pigments are gently incorporated into the paint composition. The extruder shaft illustrated only in the end area 11 has a λ homogenization on which are incorporated the elements Effektpig ¬ gently into the homogeneous coating matrix. There are also extruder with multiple extruder shafts conceivable. Figures 5a and 5b each show a sample to determine the graininess and the Sparkelingintensität an inventive powder coating layer (5a; A) and a sample of a powder ¬ lacquer layer according to the prior art by means of conventional
Einextrusion (Figur 5b; B) . Beide Proben sind mit denselben Effektpigmenten, derselben Grössenverteilung der Effektpigmente und derselben Lackrezeptur hergestellt worden. Deutlich zu erkennen ist die unterschiedliche Körnigkeit. Extrusion (Figure 5b, B). Both samples were prepared with the same effect pigments, the same size distribution of the effect pigments and the same paint formulation. Clearly recognizable is the different granularity.
Figur 6 zeigt nun den direkten Vergleich der gemessenen Graininess (Y-Achse) der Proben gemäss den Figuren 5a und 5b (X- Achse) , wobei dabei das vorgängig beschriebene Messverfahren mit Hilfe des Messgerätes BYK mac i 23 von der Fa. Altana /Byk durchgeführt wurde. Die Werte mit der Bezeichnung A entsprechen dabei denjenigen der Probe mit der erfindungsgemässen Pulverlackschicht, während die Bezeichnung B eine Pulverlackschicht nach der klassischen Einextrusion kennzeichnet. Für die Probe A wurde eine Grainisess mit einem Wert von ca. 10 für Probe B von ca. 3.5 ermittelt. FIG. 6 now shows the direct comparison of the measured graininess (Y-axis) of the samples according to FIGS. 5a and 5b (X-axis), whereby the previously described measuring method with the aid of the measuring device BYK maci 23 from Altana / Byk was carried out. The values with the designation A correspond to those of the sample with the powder coating layer according to the invention, while the designation B denotes a powder coating layer after the classical one-pass extrusion. For sample A, a Grainisess with a value of about 10 for sample B of about 3.5 was determined.
Figur 7 zeigt den direkten Vergleich der gemessenen Sparkelin- gintensitäten der Proben (Y-Achse) gemäss den Figuren 5a und 5b. Dabei wurde wiederum mit dem Messgerät BYK mac i 23 von der Fa. Altana /Byk gemessen. Dargestellt sind die Resultate der unter¬ schiedlichen Betrachtungswinkel 10°, 45°, 75° sowie deren Summe Σ (X-Achse) . FIG. 7 shows the direct comparison of the measured spark-in intensities of the samples (Y-axis) according to FIGS. 5a and 5b. Again, measurements were taken with the BYK mac i 23 measuring instrument from Altana / Byk. Shown are the results of different union among ¬ viewing angle 10 °, 45 °, 75 ° and the sum Σ (X-axis).
Figur 8a zeigt eine Probe A zur Bestimmung der Natronlaugenbe¬ ständigkeit einer erfindungsgemässen Pulverlackschicht, während Figur 8b eine solche Probe B mit einer Pulverlackschicht nach dem Stand der Technik (Einextrusion) zeigt. Im direkten Vergleich dieser Proben (gleiche Pigmenttype, gleiche Pigmentgrös- senverteilung, gleiche Lackmatrix) zeigten die nach dem erfin- dungsgemässen Verfahren hergestellten Pulverlackschicht eine signifikant verbesserte chemische Beständigkeit, insbesondere z.B. gegen Natronlauge bei aluminiumhaltigen Pigmenten oder Goldbronzen. Für Probe A entspricht die Natronlaugenbeständig¬ keit nach 30 min der Stufe 1, nach 60 min der Stufe 1, nach 90 min der Stufe 1 und nach 120 min der Stufe 1-2 (Fig. 8a) . Für Probe B entspricht die Natronlaugenbeständigkeit nach 30 min der Stufe 1-2, nach 60 min der Stufe 2, nach 90 min der Stufe 3 und nach 120 min der Stufe 4 (Fig. 8b) . Die visuelle Beurteilung im Natronlaugentest (Natronlaugenbeständigkeit) findet Anwendung wie bereits vorgängig gemäss den Qualitätsrichtlinien 631 der Gütegemeinschaft für die Stückgutbeschichtung von Bauteilen erläutert . 8a shows a sample A for determining the Natronlaugenbe ¬ permanence of an inventive powder coating layer, while Figure 8b shows such a sample B having a powder coating film according to the prior art (Einextrusion). In a direct comparison of these samples (same pigment type, same pigment size distribution, same coating matrix), the Powder coating layer produced by the process according to the invention significantly improved chemical resistance, in particular, for example, against caustic soda in aluminum-containing pigments or gold bronzes. For Sample A, the sodium hydroxide-resistant ¬ ness corresponds to 30 minutes of the step 1, after 60 min of the step 1, after 90 min, the step 1 and 120 min after the step 1-2 (FIG. 8a). For sample B, the caustic soda resistance after 30 minutes corresponds to stage 1-2, after 60 minutes stage 2, after 90 minutes stage 3 and after 120 minutes stage 4 (figure 8b). The visual assessment in the caustic soda test (caustic soda resistance) is applied as previously explained in accordance with the Quality Guidelines 631 of the Quality Assurance Association for the general cargo coating of components.
Die Figuren 9 a und b, 10 a und b und 11 a und b zeigen je eine Probe zur Bestimmung der Separationsneigung von Effektpigmenten eines Pulverlackes nach dem „dry-blend"-Verfahren (Figur 9) , nach dem „bonding"-Verfahren (Fig. 10) und nach dem erfindungs- gemässen Verfahren (Fig. 11) . Figur 9 b zeigt den Bereich des Rechtecks in Figur 9 a in vergrösserter Darstellung; der gleiche Zusammenhang besteht jeweils für die Figuren 10 a und 10 b sowie 11 a und 11 b. FIGS. 9 a and b, 10 a and b and 11 a and b each show a sample for determining the separation tendency of effect pigments of a powder coating according to the dry-blend method (FIG. 9), according to the bonding method (FIG. Fig. 10) and according to the inventive method (Fig. 11). Figure 9b shows the area of the rectangle in Figure 9a in an enlarged view; the same relationship exists for the figures 10 a and 10 b and 11 a and 11 b.
In Figur 9 a ist ein sehr deutlicher Umgriff des Pulverlackes auf die Rückseite zu erkennen. Als Umgriff versteht sich die An¬ lagerung von separierten Effektpigmenten an Kanten der Rückseite einer beschichteten Oberfläche. Die separierten Effektpigmente folgen den Feldlinien des elektrischen Felds und lagern sich daher konzentriert an den Kanten der Rückseite an. Ausserdem zeigt sich eine sehr starke Separierung zwischen Effektmittel und dem Grundpulverlack. Diese Separierung ist besonders stark auf den Kanten, des zuvor schwarzen Bleches, sichtbar. Zudem ist eine überhöhte Menge an losen Effektpigmenten auf der Oberfläche sichtbar, welche durch die nachträgliche Anhaftung von separierten Effektpigmenten entsteht. Dies wird besonders deutlich in der vergrösserten Darstellung einer Kante des Blechs in Figur 9 b. Die Kante des Blechs ist auffallend hell, was durch die Anla¬ gerung von separierten Effektpigmenten verursacht wird. In Figure 9 a is a very clear Umgriff the powder coating on the back to recognize. As wrapping is understood the An ¬ storage of separated effect pigments on edges of the back of a coated surface. The separated effect pigments follow the field lines of the electric field and therefore accumulate concentrated at the edges of the back. In addition, there is a very strong separation between the effect agent and the base powder coating. This separation is particularly visible on the edges of the previously black sheet. In addition, there is an excessive amount of loose effect pigments on the surface visible, which results from the subsequent adhesion of separated effect pigments. This is particularly clear in the enlarged view of an edge of the sheet in Figure 9 b. The edge of the sheet is remarkably light, which is caused by the delay of Appendices ¬ separated effect pigments.
Auch in den Figuren 10 a und b ist ein deutlicher Umgriff des Pulverlackes auf der Rückseite erfolgt. Sichtbar ist eine leich¬ te Separierung zwischen Effektmittel und dem Grundpulverlack. Diese ist auf den Kanten, des zuvor schwarzen Bleches, sichtbar. Eine überhöhte Menge an losen Effektpigmenten hat sich auf der Oberfläche abgeschieden, dies ist jedoch deutlich weniger stark ausgeprägt im Vergleich zu dem Dry-Blend-Pulverlack (siehe Figur 9 a und b) . Also in the figures 10 a and b a significant encroachment of the powder coating is done on the back. Visible is a facilitated separation between ¬ te effect means and the base powder paint. This is visible on the edges of the previously black sheet. An excessive amount of loose effect pigments has deposited on the surface, but this is much less pronounced compared to the dry-blend powder coating (see FIGS. 9 a and b).
In Figur 11 a erfolgte kein erkennbarer Umgriff des Pulverlackes auf der Rückseite. Es ist nahezu keine Separierung zwischen Ef¬ fektmittel und dem Grundpulverlack zu erkennen. Ausserdem ist kein Nachflittern von losen Effektpigmenten erkennbar. Dies wird besonders deutlich in der vergrösserten Darstellung einer Kante des Blechs in Figur 11 b. Die Kante des Blechs ist dunkel. Damit hat keine Separierung von Effektpigmenten vom Grundpulver stattgefunden, was zu einer Anlagerung von separierten Effektpigmenten auf der Kante hätte führen können. In FIG. 11 a, there was no discernible wraparound of the powder coating on the back. There is almost no separation between Ef ¬ fektmittel and the base powder paint to recognize. In addition, there is no noticeable fluttering of loose effect pigments. This is particularly clear in the enlarged view of an edge of the sheet in Figure 11 b. The edge of the sheet is dark. Thus, no separation of effect pigments from the base powder took place, which could have led to an accumulation of separated effect pigments on the edge.
Die Figuren 12, 13 und 14 zeigen je eine Probe zur Beurteilung der Wolken- und Streifenbildung im uneingebrannten Zustand eines Pulverlackes nach dem „dry-blend"-Verfahren (Figur 12), nach dem „bonding"-Verfahren (Figur 13) und nach dem erfindungsgemässen Verfahren (Figur 14) . Dabei wird unter standardisierten Bedingungen mit Hilfe der Automatikapplikation der Pulverlack aufgetragen . In Figur 12 ist durch die Separierung von Effektpigment und dem Grundpulverlack eine starke Wolken- und Streifenbildung entstanden. In Figur 13 ist nur noch eine leichte Wolken- und Streifenbildung zu erkennen. In Figur 14 tritt keine oder nahezu keine Separierung auf. Es sind keine Wolken und keine Streifen erkennbar . FIGS. 12, 13 and 14 each show a sample for assessing clouding and streaking in the unannoked state of a powder coating according to the dry-blend method (FIG. 12), after the bonding method (FIG. 13) and according to FIG the inventive method (Figure 14). The powder coating is applied under standardized conditions with the help of the automatic application. In FIG. 12, the separation of effect pigment and the base powder coating has resulted in strong clouding and banding. In Figure 13 only a slight cloud and banding can be seen. In Figure 14, no or almost no separation occurs. There are no clouds and no stripes.
In den Figuren 15a und b sind je eine mikroskopische Aufnahme von Pulverlack-Pulver nach dem „dry-blend"-Verfahren in unterschiedlicher Vergrösserung, 1500x (Figur 15a) und 250x (Figur 15b) dargestellt. Die Effektpigmente liegen lose verteilt - d.h. ohne Anbindung- zwischen den übrigen Pulverlackpartikeln vor. 15a and b each show a microscopic photograph of powder coating powder according to the "dry-blend" method at a different magnification, 1500x (FIG. 15a) and 250x (FIG. 15b) - Between the other powder coating particles before.
In den Figuren 16a und b sind je eine mikroskopische Aufnahme von Pulverlack-Pulver nach dem „bonding"-Verfahren in unterschiedlicher Vergrösserung, 1500x (Figur 16a) und 250x (Figur 16b) dargestellt. Die Effektpigmente sind teilweise mit Pulver¬ lackpartikeln beaufschlagt. In the Figures 16a and b is a micrograph of the powder coating powder according to the "bonding" process in different magnifications, 1500x (Figure 16a) and 250x (Figure 16b) are shown each. The effect pigments are partially charged with powder ¬ paint particles.
In den Figuren 17a und b sind je eine mikroskopische Aufnahme von Pulverlack-Pulver nach dem erfindungsgemässen Verfahren in unterschiedlicher Vergrösserung, 1500x (Figur 17a) und 250x (Figur 17b) dargestellt. Die Effektpigmente sind im Wesentlichen mit der Lackmatrix umhüllt und aus diesem Grund nur schwer zu erkennen . FIGS. 17 a and b each show a microscopic photograph of powder coating powder according to the process of the invention in a different magnification, 1500 × (FIG. 17 a) and 250 × (FIG. 17 b). The effect pigments are essentially coated with the paint matrix and therefore difficult to detect.
Die Figuren 18, 19 und 20 zeigen eine Darstellung der Rückgewinnungsstabilität nach unterschiedlichen Zeiten (15 min, 30 min, 45 min, 60 min und 75 min) eines Pulverlackes nach dem „dry- blend"-Verfahren (Figur 18), nach dem „bonding"-Verfahren (Figur 19) und eines Pulverlackes hergestellt nach dem erfindungsgemäs¬ sen Verfahren (Figur 20) . Der Farbton und die Effektstabilität werden in einem standardisierten Rückgewinnungsversuch bestimmt. „dry-blend"-Pulverlacke zeigen bereits nach einer 15 minütigen Beanspruchung im Pulverlackkreislauf deutliche Farbton und Ef¬ fektverschiebungen. Nach dem „bonding"-Verfahren hergestellte Pulverlacke zeigen nach einer 30 minütigen Beanspruchung im Pulverlackkreislauf deutliche Farbton und Effektverschiebungen. Sie sind jedoch stabiler in den Rückgewinnungseigenschaften als „dry-blend"-Pulverlacke . Die nach dem erfindungsgemässen Verfahren hergestellten Pulverlacke zeigen eine signifikant höhere Rückgewinnungsstabilität als die beiden andern Pulverlacke. Die Farbton und Effektverschiebungen sind auch nach einer Zeitdauer von 75 Minuten nur minimal zu erkennen. Für den Rückgewinnungsversuch werde beispielsweise eine Anlage und Applikationsparame¬ ter gemäss nachfolgender Tabelle verwendet. FIGS. 18, 19 and 20 show a representation of the recovery stability after different times (15 min, 30 min, 45 min, 60 min and 75 min) of a powder coating according to the dry-blend method (FIG. 18), according to FIG. bonding "method (Figure 19) and a powder coating prepared by the method erfindungsgemäs ¬ sen (Figure 20). The hue and the effect stability are determined in a standardized recovery test. "Dry-blend" powder coatings already show significant hue and Ef ¬ fektverschiebungen after a 15 minute exposure in the powder coating cycle. After the "bonding" process powder coatings prepared stress show a 30 minute in the powder coating cycle clear color tone and effect shifts. However, they are more stable in the recovery properties than dry-blend powder coatings The powder coatings prepared by the process according to the invention show a significantly higher recovery stability than the two other powder coatings For the recovery attempt, for example, a plant and application parameters are used according to the following table.
Beschreibung Gerätschaf en Description of equipment
Hersteller Automatikbeschichtungsan¬ Gema Switzerland GmbH Manufacturer Automatikbeschichtungsan ¬ Gema Switzerland GmbH
läge would
Art der Automatikbeschichtungsanlage Stahlkabine/Edelstahl  Type of automatic coating machine Steel cabin / stainless steel
Bezeichnung der AutomatikbeschichBV 01 40 - 14 - 180  Designation of automatic coating BV 01 40 - 14 - 180
tungsanlage treatment plant
Rückgewinnungseinheit Mono- Zyklon ZR1150G  Recovery Unit Mono- Cyclone ZR1150G
Absaugleistung der Rückgewinnungsein10000m 3/h Extraction power of recovery 10000m 3 / h
heit Ness
Pulverrückführung über Propfenförde- Gema Switzerland GmbH  Powder recycling via Propfenförde- Gema Switzerland GmbH
rung tion
Hersteller Pulverförderbehälter J. Wagner GmbH  Manufacturer Pulverförderbehälter J. Wagner GmbH
Bezeichnung Pulverförderbehälter L 25 Behälter  Designation Powder transport container L 25 Container
Besonderheiten Pulverförderbehälter Rundbehälter mit Fluidisierung Special features Powder transport container Round container with fluidization
Bei der Prüfung/Einfüllmenge Pulver 5000 gramm When testing / filling amount of powder 5000 grams
Pulverförderung Pumpe Inj ektor/Venturiprinzip  Powder pump Inj ector / Venturi principle
Hersteller Pulverpumpe/Applikation Gema Switzerland GmbH  Manufacturer Powder pump / application Gema Switzerland GmbH
Bezeichnung Pulverpumpe/Applikation OptiFlow IG02  Description Powder pump / application OptiFlow IG02
Bezeichnung PulverPOE- Pulverschlauch mit Erdungslitze schlauch/Applikation  Description PowderPOE powder hose with grounding hose / application
Hersteller Pulverschlauch/Applikation Huber-Suhner/Gema Switzerland GmbH Manufacturer Powder hose / application Huber-Suhner / Gema Switzerland GmbH
Innendurchmesser Pulver11 mm Inside diameter powder 11 mm
schlauch/Applikation hose / application
Länge Pulverschlauch/Applikation 8 Meter  Length of powder hose / application 8 meters
Hersteller Pulverpistole/Applikation Gema Switzerland GmbH  Manufacturer Powder gun / application Gema Switzerland GmbH
Bezeichnung Pulverpistole/Applikation OptiGun / TYP GA02  Designation Powder gun / application OptiGun / TYPE GA02
Pistolenausrüstung (Düse) /Applikation Flachstrahldüse  Gun Equipment (Nozzle) / Application Flat jet nozzle
Pistolensteuerung/Applikation OptiStar CG06  Gun control / application OptiStar CG06
Prüfmittel und Parameter  Test equipment and parameters
Prüfbleche Q- Panneis A5 / Alublech- Chromatiert Test Panels Q- Panneis A5 / Aluminum Plated - Chromated
Prüfdauer 75 Minuten Pulverausstoss für den Kreislaufbe¬ ca. 280 gramm/minute Test duration 75 minutes Powder output for the circulation ¬ about 280 grams / minute
trieb shoot
Parameter für Kreislaufbetrieb = 280 FL = 100 %, GL = 4,0m3/h, KV = ohne gr/min Circulation mode = 280 FL = 100%, GL = 4.0m 3 / h, KV = no gr / min
Beschichtung von Prüfblechen  Coating of test sheets
Start Prüfung Prüfblech mit Frischpulver nach 15 Minuten = ca. 0,8 Umläufe / Prüfblech mit Rückgewinnungspulver im Zyklon  Start test Test plate with fresh powder after 15 minutes = approx. 0.8 revolutions / test plate with recovery powder in the cyclone
nach 30 Minuten = ca . 1,7 Umläufe / Prüfblech mit Rückgewinnungspulver im Zyklon after 30 minutes = approx. 1.7 revolutions / test plate with recovery powder in the cyclone
nach 45 Minuten = ca . 2,5 Umläufe / Prüfblech mit Rückgewinnungspulver im Zyklon after 45 minutes = approx. 2.5 revolutions / test plate with recovery powder in the cyclone
nach 60 Minuten = ca . 3,4 Umläufe / Prüfblech mit Rückgewinnungspulver im Zyklon after 60 minutes = approx. 3.4 revolutions / test plate with recovery powder in the cyclone
nach 75 Minuten = ca . 4,2 Umläufe / Prüfblech mit Rückgewinnungspulver im Zyklon after 75 minutes = approx. 4.2 revolutions / test sheet with recovery powder in the cyclone
Applikationsparameter für Prüfbleche  Application parameters for test sheets
Automatikpistolen 1 x OptiGun / TYP GA02  Automatic pistols 1 x OptiGun / TYPE GA02
Förderluft (FL) 20%  Conveying air (FL) 20%
Gesamtluft (GL) 4, OrnVh  Total air (GL) 4, OrnVh
Zerstäuberluft (ZL) 0, 3m3/h Atomizing air (ZL) 0, 3m 3 / h
Hochspannung (KV) 80  High voltage (KV) 80
Strombegrenzung (μΑ) 80  Current limit (μΑ) 80
Sprühabstand 250mm  Spray distance 250mm
Hubhöhe 620mm  Lifting height 620mm
Hubgeschwindigkeit 0, 23m/sek  Lifting speed 0, 23m / sec
Transportgeschwindigkeit / Prüfblech 1 , 2m/min  Transport speed / test plate 1, 2m / min

Claims

Patentansprüche claims
1. Pulverlack in partikulärer Form mit Effektpigmenten (1), dadurch gekennzeichnet, dass die Effektpigmente (1) wenigs¬ tens zu 50%, insbesondere wenigstens zu 75%, bevorzugt we¬ nigstens zu 90% mit einer filmbildenden Lackmatrix benetzt und umhüllt sind. 1. Powder coating in particulate form with effect pigments (1), characterized in that the effect pigments (1) Wenig ¬ least 50%, especially at least 75%, preferably we ¬ nigstens to 90% are wetted with a film-forming coating matrix and wrapped.
2. Pulverlack nach Anspruch 1, dadurch gekennzeichnet, dass wenigstens 80 %, insbesondere wenigstens 90 %, bevorzugt wenigstens 95 % der Effektpigmente (1) mit der Lackmatrix benetzt sind. 2. powder coating according to claim 1, characterized in that at least 80%, in particular at least 90%, preferably at least 95% of the effect pigments (1) are wetted with the paint matrix.
3. Pulverlack nach Anspruch 1 oder 2, dadurch gekennzeichnet, dass die Grösse der Effektpigmente (1) einen Mittelwert zwischen 5 ym und 120 ym aufweisen. 3. powder coating according to claim 1 or 2, characterized in that the size of the effect pigments (1) have an average value between 5 ym and 120 ym.
4. Pulverlack nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, dass die Grösse der Effektpigmente (1) ei¬ ner Normalverteilung mit einem Mittelwert und einer Standardabweichung kleiner oder gleich 50%, insbesondere kleiner oder gleich 30%, bevorzugt kleiner oder gleich 10%, des Mittelwerts entspricht. 4. powder coating according to one of the preceding claims, characterized in that the size of the effect pigments (1) ei ¬ ner normal distribution with an average and a standard deviation less than or equal to 50%, in particular less than or equal to 30%, preferably less than or equal to 10%, of the mean.
5. Pulverlack nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, dass weniger als 40%, insbesondere weniger las 20%, bevorzugt weniger als 10%, der Effektpigmente (1) eine Bruchkante (2) aufweisen. 5. Powder coating according to one of the preceding claims, characterized in that less than 40%, in particular less las 20%, preferably less than 10%, of the effect pigments (1) have a breaking edge (2).
6. Pulverlack nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, dass der Volumenanteil der Effektpigmente (1) zwischen 1% bis 50%, insbesondere zwischen 1% bis 30%, bevorzugt zwischen 1% bis 10% vom Gesamtvolumen des Pulverlackes beträgt. 6. Powder coating according to one of the preceding claims, characterized in that the volume fraction of the effect pigments (1) is between 1% to 50%, in particular between 1% to 30%, preferably between 1% to 10% of the total volume of the powder coating.
7. Pulverlack nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, dass die Effektpigmente ausgewählt sind aus der Liste umfassend: 7. Powder coating according to one of the preceding claims, characterized in that the effect pigments are selected from the list comprising:
- Metalleffektpigmente, - metallic effect pigments,
- Perlglanzpigmente oder Interferenzpigmente, Pearlescent or interference pigments,
- Leuchtpigmente, - luminescent pigments,
- Edelstahlpigmente, - stainless steel pigments,
- Kupferpigmente, - copper pigments,
- Goldbronzepigmente - Gold bronze pigments
- Glasflakes, - glass flakes,
- Glashohlkugeln, - glass bubbles,
- Aluminiumpigmente. - Aluminum pigments.
8. Pulverlack nach einem der Ansprüche 1 bis 7, dadurch gekennzeichnet, dass eine mit dem Pulverlack hergestellte Schicht eine Natronlaugenbeständigkeit der Stufe 1 nach ei¬ ner Einwirkzeit von 30 min, der Stufe 1 bis Stufe 2 nach einer Einwirkzeit von 60 min und der Stufe 1 bis Stufe 3 nach einer Einwirkzeit von 90 min und 120 min zeigt. 8. Powder coating according to one of claims 1 to 7, characterized in that a layer produced with the powder coating a sodium hydroxide resistance of stage 1 after ei ¬ ner exposure time of 30 min, the stage 1 to stage 2 after a contact time of 60 min and the stage 1 to 3 after an exposure time of 90 minutes and 120 minutes.
9. Pulverlack nach einem der Ansprüche 1 bis 8 dadurch gekennzeichnet, dass die Lackmatrix Farbmittel aufweist. 9. Powder coating according to one of claims 1 to 8, characterized in that the paint matrix colorant.
10. Pulverlack in ausgehärteter Form hergestellt aus Pulverlack gemäss einem der Ansprüche 1 bis 9. 10. Powder coating in cured form prepared from powder coating according to one of claims 1 to 9.
11. Verfahren zur Herstellung von Pulverlack mit Effektpigmenten (1), insbesondere nach einem der Ansprüche 1 bis 9, wo¬ bei mittels eines Extruders (10) eine homogene thermoplas¬ tische Lackmasse aus den Ausgangsstoffen, insbesondere um¬ fassend Bindemittel, Additive, Farbmittel und/oder Füll¬ stoffe, hergestellt wird und die Lackmasse nach dem Verlas¬ sen des Extruders (10) vermählen wird, dadurch gekennzeichnet, dass die Effektpigmente (1) in einem Endbereich des Extruders (10) zugegeben und in der viskosen Lackmasse dis- pergiert werden. 11. A process for the preparation of powder coating with effect pigments (1), in particular according to one of claims 1 to 9, where ¬ by means of an extruder (10) a homogeneous thermoplas ¬ table lacquer composition of the starting materials, in particular to ¬ comprehensive binder, additives, colorants and / or filling ¬ substances, is prepared, and the coating mass is milled after the abandoned ¬ sen of the extruder (10), characterized in that the effect pigments (1) in an end region of the extruder (10) was added and discontinuous in the viscous paint composition be pergiert.
12. Verfahren nach Anspruch 11, dadurch gekennzeichnet, dass die Effektpigmente (1) gravimetrisch oder volumetrisch dosiert zugegeben werden. 12. The method according to claim 11, characterized in that the effect pigments (1) are added gravimetrically or volumetrically metered.
13. Verfahren nach Anspruch 11 oder 12, dadurch gekennzeichnet, dass die Effektpigmente (1) unter Schutzgas, insbesondere unter Stickstoff, zugegeben werden. 13. The method according to claim 11 or 12, characterized in that the effect pigments (1) are added under protective gas, in particular under nitrogen.
14. Verfahren nach einem der Ansprüche 11 bis 13, dadurch gekennzeichnet, dass die Ausgangsstoffe Farbmittel umfassen. 14. The method according to any one of claims 11 to 13, characterized in that the starting materials comprise colorants.
EP15700490.4A 2014-01-19 2015-01-19 Powder paint in particulate and cured form with effect pigments and process for preparing powder paint with effect pigments Active EP3094691B1 (en)

Priority Applications (2)

Application Number Priority Date Filing Date Title
PL15700490T PL3094691T3 (en) 2014-01-19 2015-01-19 Powder paint in particulate and cured form with effect pigments and process for preparing powder paint with effect pigments
EP15700490.4A EP3094691B1 (en) 2014-01-19 2015-01-19 Powder paint in particulate and cured form with effect pigments and process for preparing powder paint with effect pigments

Applications Claiming Priority (3)

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EP14151697.1A EP2896661A1 (en) 2014-01-19 2014-01-19 Powder paint in particulate and cured form with effect pigments and process for preparing powder paint with effect pigments
PCT/EP2015/050853 WO2015107181A1 (en) 2014-01-19 2015-01-19 Powder paint in particulate and hardened form having effect pigments and method for producing powder paint having effect pigments
EP15700490.4A EP3094691B1 (en) 2014-01-19 2015-01-19 Powder paint in particulate and cured form with effect pigments and process for preparing powder paint with effect pigments

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WO2015107181A1 (en) 2015-07-23
DK3094691T3 (en) 2019-07-22
EP2896661A1 (en) 2015-07-22
PL3094691T3 (en) 2019-10-31
TR201909876T4 (en) 2019-07-22

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